CAJ | 학술논문

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）2·6H2 O 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1200℃）下保温3 h 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炭的抗氧化性、物相组成和显微结构。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，Ni 掺杂酚醛树脂热解炭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50～100 nm、长度可达几十微米的多壁碳纳米管；4）在 Ar 气氛中炭化更有利于碳纳米管的生成，并且热解炭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℃。
위료제고분철수지적잔탄솔병우화열해탄적결구화성능，장 Ni（NO3）2·6H2 O 안1∶100적질량비참입열고성분철수지중제비 Ni 참잡분철수지，경200℃고화후，분별재불동기분（매탄화 Ar 기분）화불동온도（600、800、1000화1200℃）하보온3 h 탄화，연후검측기잔탄솔，병차조차시소묘량열의、X 사선연사의、능보의、소묘전경、투사전경표정기열분해특정급기열해탄적항양화성、물상조성화현미결구。결과표명：1）Ni 참잡분철수지재800화1000℃적잔탄솔균비미참잡분철수지적제고교다；2）수탄화온도적승고，Ni 참잡분철수지열해탄축점향석묵화탄결구방향연화；3）Ni 참잡분철수지경1000℃탄화형성적열해탄중유대량직경50～100 nm、장도가체궤십미미적다벽탄납미관；4）재 Ar 기분중탄화경유리우탄납미관적생성，병차열해탄구유경고적잔탄솔화결정도；5）1200℃탄화형성적열해탄적항양화성현저제고，양화봉치온도비미참잡분철수지적제고약84℃。
Ni-doped phenol resin was prepared with 1 100 mass ratio of Ni(NO3 )2 ·6H2 O 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.