氮掺杂空心碳球的制备及其光学性质研究

doi:10.15541/jim20150648

摘要/Abstract

摘要：

采用直流电弧放电法, 使用填充法制备的阳极棒, 制备了氮掺杂空心碳球(NDHCSs)。分别使用FESEM、HRTEM、EDX、EELS、XRD、UV-vis等对不锈钢片上的沉积产物进行表征, 结果表明: NDHCSs直径主要在110~543 nm, 球壁厚度在2~12 nm, 由分布比较均匀的C、N和O元素组成, 主要由石墨碳和另一种碳物相构成; 其在无水乙醇中形成的悬浮液的UV-vis吸收光谱在210 nm、221 nm和264 nm处有三个吸收峰, 在紫外光照射下呈现绿色。本文还对NDHCSs生成机理进行了简单的探讨。

关键词: 电弧放电, 氮掺杂, 空心碳球, 光学性质, 生成机理

Abstract:

N-doped hollow carbon spheres (NDHCSs) were prepared by DC arc discharge at 800℃ in nitrogen, using anode prepared by the filling method. The morphology, structure, chemical and phase compositions, and optical properties of the product deposited on the stainless steel sheet were characterized by using FESEM, HRTEM, EDX, EELS, XRD, and UV-Vis, respectively. The results show that the outer diameters of the NDHCSs are in the range of 110-543 nm and their wall thicknesses are in the range of 2-12 nm. The walls consist of two parts, namely, the inner part and the outside part, which are comparatively complete structure of graphite and discontinuously wave-like structure of layer, respectively. The NDHCSs consist of C, N and O elements with comparatively uniform distribution. The phase composition of NDHCSs mainly includes graphitic carbon and another carbon phase. The UV-Vis spectra of the suspensions of the NDHCSs in ethanol show three absorption peaks at 210 nm, 221 nm and 264 nm. Such suspension emits green luminescence under UV light irradiation and can keep stable at least for two months. The NDHCSs may have potential application in the field of optics.

Key words: arc discharge, N-doped, hollow carbon spheres, optical properties, mechanism of formation

中图分类号:

O613
TB321

胡枫香, 李玲, 林奎, 崔兰, 石彩静, Sayyar Ali Shah, 崔屾. 氮掺杂空心碳球的制备及其光学性质研究[J]. 无机材料学报, 2016, 31(8): 827-833.

HU Feng-Xiang, LI Ling, LIN Kui, CUI Lan, SHI Cai-Jing, SAYYAR Ali Shah, CUI Shen. Preparation of N-doped Hollow Carbon Spheres and Investigation of Their Optical Properties[J]. Journal of Inorganic Materials, 2016, 31(8): 827-833.

图/表 7

图1 不锈钢片表面沉积产物的FESEM照片

Fig. 1 FESEM images of the product deposited on the stainless steel sheet

图2 沉积产物的低倍HRTEM照片和EELS谱图

Fig. 2 HRTEM image and EELS Spectrum of the deposit(a) HRTEM image of the deposit at low magnification; (b) Image of the morphology corresponding to the EELS measurement; (c) EELS spectrum of the small area pointed by the arrow in (b) (the inset shouing the magnification of the N-K edge)

图3 空心球状物(a)及其1和2处球壁(b)的HRTEM照片(插图为其低倍HRTEM照片)

Fig. 3 HRTEM image of approximately spherical hollow sphere (a) and the walls pointed by the arrows 1 and 2 in (a), (b), and (c), respectively (inset showing HRTEM image of its surrounding area at low magnification)

图4 (a)放置一周后的悬浮液中的沉积产物的低倍HRTEM照片; (b)为(a)中箭头所示区域的EDX谱图

Fig. 4 (a) HRTEM image of the deposit in the suspension set for one week after ultrasonication and (b) EDX spectrum corresponding to the small area pointed by the arrow in (a)

图5 (a)空心的近似球状物的HRTEM照片以及(b~d) C、N、O的EELS元素面扫描测量结果

Fig. 5 (a) HRTEM image of the hollow and approximately spherical object and (b-d) EELS element mapping images of C, N and O, respectively

图6 不锈钢片上的沉积产物的XRD谱图

Fig. 6 XRD pattern of the product deposited on the stainless steel sheet

图7 (a)放置两个月后的上层清液和(b)再次超声分散15 min形成的悬浮液的UV-Vis吸收光谱, (c)和(d)为对应于(b)的悬浮液的光致发光性质测试的数码照片

Fig. 7 UV-Vis spectra of the samples(a) The supernatant formed after suspension being set for two months after the first ultrasonication; (b) The suspension formed after the second ultrasonication; (c-d) Digital photos for of the suspension corresponding to (b) for photoluminescent test

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