不同变质程度煤的高分辨率透射电镜分析

李霞; 曾凡桂; 司加康; 王威; 董夔; 程丽媛

不同变质程度煤的高分辨率透射电镜分析

太原理工大学煤科学与技术教育部及山西省重点实验室地球科学与工程系, 山西太原 030024

基金项目:

国家自然科学基金 41302127

国家自然科学基金 41402137

山西省煤基重点科技攻关项目 MQ2014-01

详细信息

通讯作者:
曾凡桂, Tel: 0351-6010468, E-mail: zengfangui@tyut.edu.cn

中图分类号: TQ533
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- 被引次数: 0
出版历程
- 收稿日期: 2015-10-21
- 修回日期: 2015-12-29
- 网络出版日期: 2021-01-23
- 刊出日期: 2016-03-30

High resolution TEM image analysis of coals with different metamorphic degrees

Key Laboratory of Coal Science & Technology, Ministry of Education & Shanxi Province, Department of Earth Science & Engineering, Taiyuan University of Technology, Taiyuan 030024, China

Funds:

National Natural Science Foundation of China 41302127

National Natural Science Foundation of China 41402137

Shanxi Province Coal Based Key Scientific and Technological Projects MQ2014-01

摘要

摘要: 利用高分辨率透射电子显微镜(HRTEM) 分析了三种不同变质程度煤样的结构特征.基于傅里叶-反傅里叶变换方法, 并结合Matlab、Arcgis和AutoCAD软件, 通过图像分析技术, 获得了HRTEM照片的晶格条纹参数.结果表明, 三种煤样的晶格条纹呈现不同特征, 按条纹长度分别归属于1×1-8×8共计八个类型.以3×3为临界点, 在1×1和2×2中, ML-8中芳香层片的比例高于DP-4和XM-3;在3×3-8×8中, ML-8中芳香层片的比例低于DP-4和XM-3.对比HRTEM和XRD参数d₀₀₂发现, 随着镜质组反射率的增加d₀₀₂都呈现递减趋势.
- 不同变质程度煤 /
- 高分辨率透射电子显微镜 /
- 图像分析
Abstract: The structural characteristics of 3 coals with different metamorphic degrees were analyzed using high-resolution transmission electron microscopy (HRTEM). Applying FFT-IFFT method, in association with Matlab, Arcgis and AutoCAD softwares, the lattice fringe parameters obtained from HRTEM image were determined using image analysis. The results indicate that the lattice fringes of all the test coal samples exhibit different characteristics. These lattice fringes can be divided into 8 types (1×1-8×8 aromatic fringes) according to the fringe length distribution. Taking the 3×3 aromatic fringe as critical point, the sample ML-8 abundant in 1×1 and 2×2 aromatic fringes while short of 3×3-8×8 aromatic fringes when comparing with sample DP-4 and sample XM-3. The values of d₀₀₂ obtained from both HRTEM and XRD show a decreasing trend with increasing vitrinite reflectance.
- different metamorphic degree of coal /
- high resolution transmission electron microscopy /
- image analysis

HTML全文

图 1 煤样(DP-4) 的图像解析流程

Figure 1 Diagram of image processing on lattice image of coal (DP-4)

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图 2 二值化图像的晶格边缘画线提取

Figure 2 Line drawing extraction of lattice fringe of binarization image

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图 3 煤样的XRD谱图

Figure 3 XRD spectra of coal samples

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图 4 煤样的晶格条纹特征

Figure 4 Characteristics of fringe-extracted of coal

(a₁)、(b₁)、(c₁): criginal HRTEM images; (a₂)、(b₂)、(c₂): line drawing extraction of lattice fringe; (a₃)、(b₃)、(c₃): the lattice fringe length distribution

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图 5 三个煤样芳香层片的比例分布

Figure 5 Distribution of the proportions of aromatic layer in 3 coal samples

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图 6 三个煤样XRD和HRTEM的d₀₀₂对比图

Figure 6 d₀₀₂ comparison of the XRD and HRTEM for 3 coal samples

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表 1 样品的化学和光学参数

Table 1 Chemical and optical parameters for studied samples

Samples no.	Coal mine	Proximate analysis w/%			R_{o, max} /%	Ultimate analysis w_daf/%
Samples no.	Coal mine	M_ad	A_ad	V_daf	R_{o, max} /%	C	H	O^*	N	S
DP-4	Dongpo	1.50	14.27	40.35	0.573	77.89	4.39	13.51	1.16	2.86
ML-8	Malan	0.48	9.00	27.96	1.205	86.32	4.04	6.76	1.11	1.66
XM-3	Ximing	0.70	8.18	15.18	1.838	90.43	3.73	3.95	1.08	0.72
^*: by difference

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表 2 煤样的微晶结构参数

Table 2 Microcrystalline structure parameters of coal

Sample	d₀₀₂ /nm	L_c/nm	L_a /nm
DP-4	0.373 2	1.238 6	1.011 9
ML-8	0.354 6	1.749 1	1.232 4
XM-3	0.349 5	1.952 1	1.419 1

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表 3 高分辨透射电子显微镜晶格条纹归属分类^[11]

Table 3 Classification of HRTEM lattice fringes

Aromatic sheet	Mean d/nm	Grouping d/nm
1×1	0.39	0.30-0.54
2×2	0.60	0.55-0.74
3×3	0.93	0.75-1.14
4×4	1.27	1.15-1.44
5×5	1.60	1.45-1.74
6×6	1.94	1.75-2.04
7×7	2.28	2.05-2.44
8×8	2.61	2.45-2.84

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