氧化铌/木质活性碳纤维复合材料的结构性能表征

doi:10.3969/j.issn.1673-5854.2021.02.003

摘要/Abstract

摘要：

以木质活性碳纤维（ACHF）为载体，通过浸渍草酸铌以及改变煅烧温度，制备出不同煅烧温度（400、600和800℃）下的氧化铌/木质活性碳纤维（Nb₂O₅/ACHF）。采用扫描电镜（SEM）、X射线衍射（XRD）、X光电子能谱（XPS）和全自动比表面积与孔径分析（BET）仪对制备的氧化铌/木质活性碳纤维结构、表面孔径等进行表征，并初步分析了其电化学性能。研究结果表明：随着煅烧温度的升高，纤维表面生成的正交晶型氧化铌晶体颗粒晶型越好，颗粒直径越大，且表面官能团的C—C键逐渐减少，而C—O键随之增加，比表面积从1 476.65 m²/g（400℃）降至1 302.31 m²/g（800℃），微孔率下降了10.79个百分点。此外，制备的氧化铌/木质活性碳纤维具有极好的双电层电容和赝电容特性，800℃煅烧的样品Nb₂O₅/ACHF-800表面具有多级孔隙结构，有利于其电化学性能，在电流密度为1 A/g的KOH电解液中比电容可达155 F/g。

关键词: 木质活性碳纤维, 氧化铌, XPS, 比表面积, 比电容

Abstract:

Niobium oxide/wood activated carbon fiber (Nb₂O₅/ACHF) at different calcination temperatures(400, 600 and 800 ℃) was prepared by impregnating niobium oxalate and changing calcination temperature with wood activated carbon fiber as support. The structure, surface pore size and so on of the as-prepared niobium oxide/wood activated carbon fiber were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), X-ray electron spectroscopy (XPS) and fully automatic surface area and pore size analysis (BET), and the electrochemical performance was preliminarily analyzed. The results showed that as the calcination temperature increased, the crystal form of the orthogonal niobium oxide crystal on the surface of the fiber became better, and the particle diameter became larger. The C-C bond content of the surface functional group decreased gradually, and the C-O bond increased, The specific surface area decreased from 1 476.65 m²/g(400 ℃) to 1 302.31 m²/g(800 ℃). The micropore rate decreased by 10.79 percent. In addition, the prepared niobium oxide/wood activated carbon fiber had excellent double layer capacitance and pseudocapacitance properties. The Nb₂O₅/ACHF-800 surface of 800 ℃ calcined sample had multistage pore structure. In favor of its electrochemical performance, the specific capacitance was up to 155 F/g in KOH electrolyte with the current density of 1 A/g.

Key words: wood activated carbon fiber, niobium oxide, XPS, specific surface area, specific capacitance

中图分类号:

TQ35
TQ424

刘鑫, 马晓军. 氧化铌/木质活性碳纤维复合材料的结构性能表征[J]. 生物质化学工程, 2021, 55(2): 16-22.

Xin LIU, Xiaojun MA. Structural Properties of Niobium Oxide/Woody Activated Carbon Fiber Composites[J]. Biomass Chemical Engineering, 2021, 55(2): 16-22.

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样品 sample	C1s	O1s	N1s	Nb3d
ACHF	91.87	7.71	0.42	0
Nb₂O₅/ACHF-400	84.45	12.30	0.83	1.43
Nb₂O₅/ACHF-600	86.29	11.26	0.56	1.8
Nb₂O₅/ACHF-800	85.9	11.95	1.05	1.09

样品 sample	C—C		C—O		C＝O		COOH
样品 sample	结合能/eV binding energy	百分比/% percentage	结合能/eV binding energy	百分比/% percentage	结合能/eV binding energy	百分比/% percentage	结合能/eV binding energy	百分比/% percentage
ACHF	284.6	49.57	285.2	26.99	286.8	7.72	289.1	15.72
Nb₂O₅/ACHF-400	284.6	56.37	285.1	31.09	286.7	5.46	289.1	7.08
Nb₂O₅/ACHF-600	284.6	41.00	285.1	36.62	286.6	6.77	289.1	15.61
Nb₂O₅/ACHF-800	284.6	26.89	285.1	43.57	286.6	7.96	289.0	21.58

样品 sample	比表面积/ (m²·g^-1) specific surface area	微孔表面积/ (m²·g^-1) micropore surface area	总孔容/ (cm³·g^-1) total pore volume	微孔孔容/ (cm³·g^-1) micropore volume	中孔孔容/ (cm³·g^-1) mesopore volume	微孔率/% micropore volume ratio	平均孔径/nm average pore size
ACHF	2040.88	893.72	1.05	0.47	0.30	44.83	20.43
Nb₂O₅/ACHF-400	1476.65	903.41	0.79	0.49	0.20	61.73	21.16
Nb₂O₅/ACHF-600	1369.14	781.05	0.74	0.42	0.20	57.74	22.26
Nb₂O₅/ACHF-800	1302.31	658.13	0.70	0.36	0.23	50.94	22.38

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