微螺旋炭纤维的制备与表征

doi:10.3724/SP.J.1077.2012.00541

摘要/Abstract

摘要：

采用溶剂热法合成出硫化镍, 并将其作为催化剂, 催化热解乙炔制备出微螺旋炭纤维. 通过SEM、FT-IR和XRD分析了催化剂和微螺旋炭纤维的形貌和微观结构. 结果表明: 硫化镍催化颗粒表面光滑、为规则的六方相结构, 直径为1~2 μm; 微螺旋炭纤维具有双螺旋结构, 截面为矩形, 具有相同的螺径. 微螺旋炭纤维分子结构中既含有不饱和的C=C双键, 又含有饱和的-CH₂-和-CH₃基团, 其微观结构整体有序度较差, 存在一定量的无定型炭和晶体缺陷, 石墨化度低.

关键词: 微螺旋炭纤维, 溶剂热, 硫化镍, 微观结构, 催化热解

Abstract:

Carbon microcoils (CMCs) were synthesized by the catalytic decomposition of acetylene using nickel sulfide particles as the catalyst which prepared by solvothermal method. The morphology and microstructure of the catalyst and micro-coiled carbon fibers were examined by SEM, FT-IR and XRD. The results showed that the catalyst was regular hexagonal phase nickel sulfide with its diameter of 1-2 μm and a smooth surface. CMCs have double helix structure, rectangular cross-section and identical coil diameter. The molecular structure of CMCs contained both unsaturated –C=C– and saturated –CH₂– and –CH₃ groups. The microstructure of CMCs was of poor degree of order with a low graphitization degree, containing a certain amount of amorphous carbon and crystal defects.

Key words: carbon microcoils, solvothermal, nickel sulfide, microstructure, catalytic decomposition

中图分类号:

TQ342

李宁, 寇开昌, 晁敏, 张冬娜, 吴广磊, 马利鹏. 微螺旋炭纤维的制备与表征[J]. 无机材料学报, 2012, 27(5): 541-544.

LI Ning, KOU Kai-Chang, CHAO Min, ZHANG Dong-Na, WU Guang-Lei, MA Li-Peng. Preparation and Characterization of Micro-coiled Carbon Fibers[J]. Journal of Inorganic Materials, 2012, 27(5): 541-544.

图/表 6

图1 硫化镍催化剂的SEM照片(a)和XRD图谱(b)

Fig. 1 (a) SEM image and (b) XRD pattern of NiS particles

图2 为了进一步提高微螺旋炭纤维的质量和产量, 通入适量的噻吩(通过C2H2载入噻吩作为助催化剂), C2H2的流量为10 sccm, 远小于已报道的量[14]. 图3为最佳条件下(最佳反应条件为: 反应温度750℃,气体总流量(N2、H2和C2H2)为110 sccm, 反应时间为90 min, 产率几乎为100%)制备的微螺旋炭纤维的扫描电镜照片, 由图中可以看出, 微螺旋炭纤维是由两根炭纤维规则的螺旋缠绕而成, 螺旋直径在5~10 μm, 纤维直径在1 μm左右, 螺旋管长度为毫米级, 其纤维截面为矩形, 而且其螺径和螺距都比较均匀, 螺旋缠绕的紧密程度也大致相同.

Fig. 2 SEM image of the CMCs prepared without thiophene

图3 最佳条件下制备的微螺旋炭纤维(a)低倍和(b)高倍SEM照片

Fig. 3 (a) Low and (b) high magnification SEM images of the CMCs prepared under optimal conditions

图4 不同反应温度的微螺旋炭纤维的形貌

Fig. 4 Morphologies of micro-coiled carbon fibers prepared at different temperatures (a) 700℃; (b) 750℃; (c) 800℃

图5 微螺旋炭纤维的红外图谱

Fig. 5 FT-IR spectrum of micro-coiled carbon fibers

图6 微螺旋炭纤维XRD图谱

Fig. 6 XRD pattern of micro-coiled carbon fibers

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