微晶石墨氧化-膨胀过程中微形貌与结构变化

孙红娟; 刘波; 彭同江; 段佳琪

doi:10.3799/dqkx.2018.407

微晶石墨氧化-膨胀过程中微形貌与结构变化

doi: 10.3799/dqkx.2018.407

1.
西南科技大学固体废物处理与资源化教育部重点实验室, 四川绵阳 621010
2.
西南科技大学分析测试中心, 四川绵阳 621010

基金项目:

西南科技大学龙山学术人才科研支持计划 17LZXT11

国家自然科学基金项目 41772036

国家自然科学基金项目 U1630132

详细信息

作者简介:
孙红娟(1976-), 女, 教授, 博士, 主要从事矿物材料的晶体化学及应用研究

中图分类号: P57
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- 被引次数: 0
出版历程
- 收稿日期: 2017-10-01
- 刊出日期: 2018-05-15

Micromorphology and Structure Changes of Microcrystalline Graphite during Process of Oxidation and Expansion

1.
Key Laboratory of Ministry of Education for Solid Waste Treatment and Resource Recycle, Southwest University of Science and Technology, Mianyang 621010, China
2.
Analytical and Testing Center, Southwest University of Science and Technology, Mianyang 621010, China

摘要

摘要: 为深度揭示微晶石墨氧化和膨胀过程中结构的变化规律，分别采用SEM-EDS、XRD、Raman和FTIR等测试分析手段对其产物结构进行表征研究.结果表明：微晶石墨经氧化后，层间域被撑大，结构层上接入大量的羟基、羧基和环氧基等亲水性含氧官能团.随氧化剂（KMnO₄）用量增加，产物层间距、结构缺陷和无序度逐渐增大.高温膨胀后，氧化微晶石墨被还原，结构中的部分吸附水和含氧官能团被除去，结构缺陷与无序度减小，部分sp²区域得到了恢复.膨胀微晶石墨颗粒含有丰富的网络型孔隙结构，孔径集中在2~5 nm.
- 微晶石墨 /
- 氧化 /
- 膨胀 /
- 结构 /
- 矿物学
Abstract: In order to reveal the structure changes of microcrystalline graphite in the process of oxidation and expansion, the products were characterized by means of SEM-EDS, XRD, Raman and FTIR in this study. The results show that the interlayer distance of microcrystalline graphite oxide is enlarged and many functional groups including hydroxyl, carboxyl and epoxy groups are bonded on the graphene layer in the oxidation process. In addition, with the increase of oxidant (KMnO₄), the space distance, structural defects and disorder of oxidized product increased gradually. After being expanded with high temperature, some of the oxygen-containing functional groups in the structure were removed, and the oxidized microcrystalline graphite was reduced partly. In addition, the structural defects and disorder degrees of expanded microcrystalline graphite reduced, and local sp² regions were recovered. The expanded microcrystalline graphite particles contained abundant network pore structures with pore sizes of 2-5 nm.
- microcrystalline graphite /
- oxidation /
- expansion /
- structure /
- mineralogy

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图 1 HJC-C-nKP系列样品经高温膨胀后的照片

Fig. 1. Pictures of HJC-C-nKP samples after high temperature expansion

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图 2 膨胀微晶石墨样品的SEM图

a.HJC-C-1.2P样品的SEM图；b.HJC-C-1.2P样品的SEM图选区放大图；c.HJC-C-1.6P样品的SEM图；d.HJC-C-1.6P样品的SEM图选区放大图

Fig. 2. SEM of expanded microcrystalline graphite samples

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图 3 样品HJC-C-1.6P的氮气脱吸附曲线(a)与BJH孔径分布曲线(b)

Fig. 3. N₂ adsorption-desorption isotherms (a) and pore size distributions calculated by BHJ method (b) of HJC-C-1.6P

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图 4 微晶石墨氧化(a)和膨胀(b)后产物XRD图

Fig. 4. XRD of oxidized microcrystalline graphite samples (a) and expanded microcrystalline graphite samples (b)

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图 5 微晶石墨氧化(a)和膨胀(b)后产物FTIR图

Fig. 5. FTIR of oxidized microcrystalline graphite samples (a) and expanded microcrystalline graphite samples (b)

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图 6 微晶石墨氧化(a)和膨胀(b)后产物Raman图

Fig. 6. Raman diagrams of oxidized microcrystalline graphite samples (a) and expanded microcrystalline graphite samples (b)

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表 1 各膨胀微晶石墨样品的比表面积和孔容

Table 1. The specific surface areas and pore capacity of expanded microcrystalline graphite samples

样品名称	BET比表面积(m²/g)	孔容(cm³/g)	平均孔径(nm)
HJC-C-0.4P	59.88	—	—
HJC-C-0.8P	65.89	—	—
HJC-C-1.2P	137.53	—	—
HJC-C-1.6P	189.75	1.02	29.33
注：“—”表示未检测.

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表 2 样品的FTIR谱图中官能团类型及波数

Table 2. The type of functional group and the wavenumbers in the FTIR

官能团类型	C-OH		C=C	C=O	C-O	C-O-C	H₂O(OH)
官能团类型	ν	β	ν	ν	ν	ν	ν	β
波数(cm^-1)	1 048, 1 090	1 384	1 578, 1 462	1 739	1 270	880, 1 120	3 434	1 631

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表 3 HJC-C-nKP系列和HJC-C-nP系列样品的Raman光谱参数

Table 3. Raman spectral parameters of HJC-C-nKP and HJC-C-nP samples

样品编号	D峰(cm^-1)		G峰(cm^-1)		峰间距(cm^-1)	I_D/I_G
样品编号	峰位	半峰宽	峰位	半峰宽	峰间距(cm^-1)	I_D/I_G
HJC-C	1 352.21	38.01	1 581.53	22.00	229.32	0.43
HJC-C-0.4KP	1 350.05	86.45	1 589.12	47.78	239.07	1.07
HJC-C-0.8KP	1 349.50	93.30	1 590.34	52.27	240.84	1.14
HJC-C-1.2KP	1 351.20	115.96	1 589.39	65.75	238.19	1.29
HJC-C-1.6KP	1 354.96	130.20	1 587.16	74.78	232.20	1.44
HJC-C-0.4P	1 356.43	70.79	1 583.27	30.92	226.84	0.88
HJC-C-0.8P	1 356.61	69.51	1 589.80	54.40	233.19	1.15
HJC-C-1.2P	1 355.10	89.74	1 586.34	54.18	231.24	1.15
HJC-C-1.6P	1 355.29	123.53	1 588.52	67.38	233.23	1.40

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