以乙酰丙酮铁为催化剂源,三甘醇为溶剂,通过溶剂热法在碳纤维表面负载催化剂前驱体,在 H2与 N2中一定温度下进行还原,采用化学气相沉积法在碳纤维表面生长碳纳米管。研究了催化剂的负载条件和碳纳米管的生长条件,采用 XRD、FTIR、RAMAN对乙酰丙酮铁在三甘醇中反应在碳纤维表面负载催化剂前驱体产物进行分析,用 SEM、TEM对催化剂前驱体粒子及碳纳米管的形貌进行表征。结果表明:催化剂前驱体为粒径30 nm左右的Fe3 O4颗粒,当催化剂的还原温度为415℃、还原时间为60 min时,Fe3 O4颗粒还原成纳米 Fe颗粒;当碳纳米管的生长温度为750℃、生长时间为30 min、气流体积比为V(N2)∶V(H2)∶V(C2 H2)=50∶10∶10时能在碳纤维表面生长出形貌均一、管径为30~60 nm的碳纳米管。
The homogeneous carbon nanotubes(CNTs)grown on the carbon fiber surface were synthesized by chemical vapor deposition (CVD)using Fe nanoparticles as catalyst.The Fe catalyst nanoparticles were obtained through a solvothermal reaction,where iron(Ⅲ)acetylacetone as catalytic source and triethylene glycol as solvent, and then followed by a hydrothermal reduction using mixed nitrogen and hydrogen gas flow at appropriate tempera-ture.The optimum growth condition of CNTs was systematically investigated.XRD,FTIR,RAMAN were used to analyze the products of iron(Ⅲ)acetylacetone in triethylene glycol.SEM and TEM were further employed to charac-terize catalytic precursor particles and CNTs.The results indicate that the catalytic precursors are magnetite nanopar-ticles with diameter of ca.30 nm,which can be hydrothermally reduced to iron nanoparticles at 415 ℃ for 60 min. The optimum growth parameters of the CNTs are that the growth temperature is 750 ℃ for 30 min with gas flow ratio of N2∶H2∶C2 H2 equal to 50∶10∶10.The diameter of the CNTs grown on the carbon fiber surface ranges from 30 nm to 6 0 nm.
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