煤基炭泡沫孔结构调控

doi:10.15541/jim20150628

无机材料学报 ›› 2016, Vol. 31 ›› Issue (9): 961-968.DOI: 10.15541/jim20150628

煤基炭泡沫孔结构调控

徐国忠^1,2, 金文武¹, 曾燮榕², 邹继兆², 熊信柏², 黄麟², 赵振宁¹

(1. 辽宁科技大学化工学院, 辽宁省先进煤焦化技术重点实验室, 鞍山 114051, 2. 深圳大学材料学院, 深圳市特种功能材料重点实验室, 深圳陶瓷先进技术工程实验室, 深圳 518060)

收稿日期:2015-12-14 修回日期:2016-01-27 出版日期:2016-09-20 网络出版日期:2016-08-29
作者简介:徐国忠(1973–), 男, 副教授. E-mail: gz_xu@163.com
基金资助:
国家自然科学基金(51272161, 51202150);辽宁省教育厅项目(L2013124);辽宁科技大学专项基金(2012YY03)

Tailoring of Pore Structure of Coal-based Carbon Foam

XU Guo-Zhong^1,2, JIN Wen-Wu¹, ZENG Xie-Rong², ZOU Ji-Zhao², XIONG Xin-Bai², HUANG Lin², ZHAO Zhen-Ning¹

(1. Liaoning Key Laboratory of Advanced Coal and Coking Technology, College of Chemical Engineering, University of Science and Technology Liaoning, Anshan 114051, China; 2. Shenzhen Key Laboratory of Special Functional Materials & Shenzhen Engineering Laboratory for Advance Technology of Ceramics, College of Materials Science and Engineering, Shenzhen University, Shenzhen 518060, China)

Received:2015-12-14 Revised:2016-01-27 Published:2016-09-20 Online:2016-08-29
About author:XU Guo-Zhong. E-mail: gz_xu@163.com
Supported by:
National Natural Science Foundation of China (51272161, 51202150);Liaoning Provincial Education Department Foundation (L2013124);Special Foundation of University of Science and Technology Liaoning (2012YY03)

摘要/Abstract

摘要：

以肥煤镜质组富集物为前驱体, 采用高压渗氮法制备煤基炭泡沫, 研究了发泡温度、发泡压力和发泡时间对炭泡沫孔结构的影响。利用SEM观察炭泡沫的孔胞形貌, 同时利用Nano Measurer分析软件统计SEM照片孔胞直径分布和孔喉直径分布以及平均孔径。结果表明: 微孔塑料成核理论可以定性解释炭泡沫的孔结构变化趋势。发泡温度的升高导致成核密度增加, 同时导致气体在胶质体的溶解度降低, 不利于孔胞长大。发泡压力的增大导致炭泡沫的孔胞密度增加, 临界成核半径降低, 同时加剧了热聚合反应, 导致胶质体的粘度增大, 不利于孔胞长大。发泡时间的延长会使热聚合更加充分, 影响胶质体粘度, 进而影响孔结构。

关键词: 炭泡沫, 孔结构, 成核理论, 煤

Abstract:

Vitrinite-concentration of fat coal was used as precursor to prepare carbon foams by nitrizing under high pressure. Influences of foaming temperature, pressure and time on the pore structure of carbon foams were investigated, whose prarameters include bulk density, porosity, morphology, pore cell average diameter, and the distribution of pore cell diameter and pore throats. The morphology of pore cell was observed by SEM. The distributions of pore cell diameters and pore throats as well as the mean diameter were calculated using analytical software of Nano Measurer 1.2. Results show that the nucleation of microcellular thermoplastic foam can qualitatively reveal the variable trend of pore cell structure of carbon foams. Rising of the foaming temperature results in nucleation volume density enhancement. Meanwhile, the rising temperature reduces the gas solubility in plastic mass, which is not conducive to the cell growth. Increasing foaming pressure leads to pore cell density enhancement, whereas the critical nucleation radius decrease. In addition, the increased foaming pressure exacerbates thermal polymerization reaction, increasing viscosity of the plastic mass, which is not conducive to the growth of pore cell. Extending foaming time enables thermal polymerization more sufficiently, which influences the viscosity of the plastic mass and further affects the pore structure.

Key words: carbon foam, pore structure, nucleation theory, coal

中图分类号:

TQ383

徐国忠, 金文武, 曾燮榕, 邹继兆, 熊信柏, 黄麟, 赵振宁. 煤基炭泡沫孔结构调控[J]. 无机材料学报, 2016, 31(9): 961-968.

XU Guo-Zhong, JIN Wen-Wu, ZENG Xie-Rong, ZOU Ji-Zhao, XIONG Xin-Bai, HUANG Lin, ZHAO Zhen-Ning. Tailoring of Pore Structure of Coal-based Carbon Foam[J]. Journal of Inorganic Materials, 2016, 31(9): 961-968.

图/表 16

表1 肥煤及其镜质组富集物的工业分析和元素分析结果

Table 1 Proximate analysis and ultimate analysis of the fat coal and its vitrinite-concentration

precursors	Proximate analysis /wt%			Ultimate anasysis/wt%
precursors	M_ad	A_d	V_daf	C	H	O	N	S
Fat coal	1.6	8.52	38.29	88.16	4.92	4.84	1.46	0.62
Vitrinite	1.7	3.50	43.80	86.45	5.73	5.65	1.53	0.64

图1 前驱体的TG和DTG曲线

Fig. 1 TG and DTG curves of the precursor

图2 前驱体基氏流动度自然对数与温度的关系

Fig. 2 Correlation between LNF and temperature

图3 碳泡沫制备装置示意图

Fig. 3 Schematic diagram of the oxperimental set-up

图4 捣固压力对炭泡沫体密度和气孔率的影响

Fig. 4 Effect of the stamping pressure on the bulk density and porosity of carbon foams

图5 捣固压力对炭泡沫孔泡形貌的影响

Fig. 5 Effect of stamping pressure on the pore cell morphology of carbon foams (a) 2 MPa; (b) 6 MPa; (c) 10 MPa; (d) 14 MPa

图6 捣固压力对炭泡沫孔胞直径分布(a)、孔喉直径分布(b)及平均孔胞直径(c)的影响

Fig. 6 Influence of stamping pressure on pore cell diameter distribution (a), pore throat distribution (b) and mean cell diameter (c)

图7 发泡温度对炭泡沫体密度和气孔率的影响

Fig. 7 Effect of foaming temperature on the bulk density and porosity of carbon foams

图8 不同发泡温度下炭泡沫的孔胞SEM照片

Fig. 8 Influence of foaming temperature on the pore cell morphology of carbon foams(a) 393℃; (b) 413℃; (c) 433℃; (d) 453℃; (e) 473℃

图9 发泡温度对炭泡沫孔胞直径分布(a)、孔喉直径分布(b)及孔胞的平均直径(c)的影响

Fig. 9 Influence of foaming temperature on pore cell diameter distribution (a), pore throat distribution (b) and mean cell diameter (c) of carbon foams

图10 发泡压力对炭泡沫体密度和气孔率的影响

Fig. 10 Effect of foaming pressure on the bulk density and porosity of carbon foams

图11 不同发泡压力下炭泡沫孔胞的SEM照片

Fig. 11 Effect of foaming pressure on pore cell morphology of carbon foams(a) 0 MPa; (b) 2 MPa; (c) 4 MPa; (d) 6 MPa; (e) 8 MPa

图12 发泡压力对炭泡沫孔胞直径分布(a)、孔喉直径分布(b)及平均孔胞直径(c)的影响

Fig. 12 Effect of foaming pressure on pore cell diameter distribution (a), pore throat distribution diameter (b) and mean cell diameter (c) of carbon foams

图13 发泡时间对炭泡沫体密度和气孔率的影响

Fig. 13 Effect of foaming time on the bulk density and porosity of carbon foams

图14 不同发泡时间的炭泡沫孔胞SEM照片

Fig. 14 Influence of the foaming time on cell morphology of carbon foams(a) 0.5 h; (b) 1 h; (c) 2 h; (a) 2.5 h

图15 发泡时间对炭泡沫孔胞直径分布(a)、孔喉直径分布(b)和孔胞平均直径(c)的影响

Fig. 15 Effect of foaming time on pore cell diameter distribution (a), pore throat distribution (b) and mean cell diameter (c) of carbon foams

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煤基炭泡沫孔结构调控

Tailoring of Pore Structure of Coal-based Carbon Foam

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