静电纺丝制备磁性碳纳米复合纤维及其表征

doi:10.15541/jim20130577

摘要/Abstract

摘要：

以聚丙烯腈(PAN)、乙酰丙酮铁(AAI)、N, N-二甲基甲酰胺(DMF)为原料, 采用静电纺丝-煅烧技术成功制备出磁性碳纳米复合纤维。通过TEM分析发现CF900的直径约为130~210 nm, 磁性纳米颗粒均匀地分散在碳纳米纤维中, 并探讨了碳化温度对碳纳米复合纤维磁性能的影响。结果显示: 饱和磁化强度(M_s)和剩余磁化强度(M_r)均随温度的升高而增大, 样品CF900的饱和磁化强度(M_s)高达27.55 A·m²/kg, 比表面积(S_BET)和总孔容积(V_total)达354.0 m²/g和0.315 mL/g。

关键词: 静电纺丝, 碳纳米复合纤维, 磁性纳米颗粒, 磁性能

Abstract:

Magnetic carbon composite nanofibres, using the mixed homogeneous solution consist of polyacrylonitrile (PAN), ferric acetylacetonate (AAI) and dimetbylformamide (DMF) as raw material, were prepared by electrospinning-calcination technology. TEM analysis showed that the carbon nanofibre diameter of sample CF900 was about 130-210 nm, in which magneticnanoparticles were uniformly distributed. The magnetic properties of carbon composite nanofibres under different carbonization temperature was also investigated. Results showed that saturation magnetization (M_s) and remanent magnetization (M_r) increased with the increase of the temperature. When carbonization temperature was 900 ℃, the sample was of good magnetic property with high saturation magnetization (M_s=27.55 A·m²/kg). Moreover, the specific surface area (S_BET) and total pore volume (V_total) were up to 354.0 m²/g and 0.315 mL/g, respectively.

Key words: electrospinning, carbon composite nanofibres, magnetic nanoparticle, magnetic property

中图分类号:

TQ174

汤营茂, 缪清清, 肖荔人, 钱庆荣, 陈庆华. 静电纺丝制备磁性碳纳米复合纤维及其表征[J]. 无机材料学报, 2014, 29(8): 827-834.

TANG Ying-Mao, MIAO Qing-Qing, XIAO Li-Ren, QIAN Qing-Rong, CHEN Qing-Hua. Preparation and Characterization of Electrospun Magnetic Carbon Composite Nanofibres[J]. Journal of Inorganic Materials, 2014, 29(8): 827-834.

图/表 11

图1 PAN/AAI复合纳米纤维(空气氛围)(a)和预氧化后的碳纳米复合纤维(氮气氛围) (b)的DSC-TGA曲线

Fig. 1 DSC-TGA results for (a) PAN/AAI composite nanofiber in the air; (b) composite nanofiber after stabilizing treatment under the nitrogen

图2 PAN/AAI复合纳米纤维(a1, a2)和磁性碳纳米复合纤维CF900(b1, b2)的SEM照片

Fig. 2 SEM images of as spun PAN/AAI composite nanofiber (a1, a2) and magnetic carbon composite nanofiber of CF900 (b1, b2)

图3 磁性碳纳米复合纤维的高倍透射电镜照片

Fig. 3 HRTEM images of magnetic carbon composite nanofiber

图4 磁性碳纳米复合纤维的X射线能谱分析图

Fig. 4 EDS spectrum of magnetic carbon composite nanofiber

图5 各磁性纳米复合材料的XRD图谱

Fig. 5 XRD patterns of the samples

图6 各磁性碳纳米复合材料的拉曼光谱图

Fig. 6 Raman spectra of various samples

表1 各样品的石墨化程度R值的大小和石墨晶体晶面的La的大小

Table 1 The R values (R=IG/ID, degree of graphitization) of the carbon fibers and La values (La≈4.4×R) of various nanofibers

Sample	R	L_a/nm
CF500	0.84	3.70
CF600	0.92	4.05
CF700	0.93	4.09
CF800	1.02	4.49
CF900	0.94	4.14

图7 各磁性碳纳米复合材料的氮气吸脱附曲线(实心符号: 吸附支, 空心符号: 脱附支)

Fig. 7 N2 adsorption-desorption isotherms of (a) CF500; (b) CF600; (c) CF700, CF800; (d) CF900 (Closed symbol: adsorption, open symbol: desorption

表2 碳纳米复合纤维的表面积和孔容

Table 2 Surface areas and pore volumes of various magnetic carbon nanofibers

Sample ID	S_BET/(m²·g^-1)	V_total/(mL·g^-1)	D_P/nm	NLDFT
Sample ID	S_BET/(m²·g^-1)	V_total/(mL·g^-1)	D_P/nm	V_t/(mL·g^-1)	V_mic/(mL·g^-1)	V_mes/(mL·g^-1)
CF500	10.0	0.031	12.2	0.030	0.002	0.028
CF600	48.8	0.099	8.15	0.096	0.010	0.086
CF700	351.1	0.317	3.61	0.302	0.110	0.192
CF800	400.1	0.328	3.28	0.308	0.129	0.179
CF900	354.0	0.315	3.56	0.296	0.120	0.176

图8 CF500、CF600、CF700(a)和CF800、CF900(b)的磁滞回线图

Fig. 8 Magnetic hysteresis loops of (a) CF500, CF600, CF700 and (b) CF800, CF900

表3 各磁性碳纳米复合纤维在298 K下的Ms、Mr和Hc值

Table 3 Ms, Mr and Hc of magnetic carbon composite nanofibres at 298 K

Sample	M_s/(A·m²·kg^-1)	M_r/(A·m²·kg^-1)	H_c/(kA·m^-1)
CF500	1.02	0.05	7.96
CF600	7.83	0.83	7.96
CF700	16.57	3.53	16.00
CF800	22.87	4.65	19.90
CF900	27.55	5.10	19.90

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