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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

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[J]. 燃料化学学报(中英文), 2016, 44(3): 279-286.
引用本文: 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[J]. 燃料化学学报(中英文), 2016, 44(3): 279-286.
LI Xia, ZENG Fan-gui, SI Jia-kang, WANG Wei, DONG Kui, CHENG Li-yuan. High resolution TEM image analysis of coals with different metamorphic degrees[J]. Journal of Fuel Chemistry and Technology, 2016, 44(3): 279-286.
Citation: LI Xia, ZENG Fan-gui, SI Jia-kang, WANG Wei, DONG Kui, CHENG Li-yuan. High resolution TEM image analysis of coals with different metamorphic degrees[J]. Journal of Fuel Chemistry and Technology, 2016, 44(3): 279-286.

不同变质程度煤的高分辨率透射电镜分析

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

High resolution TEM image analysis of coals with different metamorphic degrees

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: 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.
  • 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)

    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

    图  3  煤样的XRD谱图

    Figure  3  XRD spectra of coal samples

    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

    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

    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

    表  1  样品的化学和光学参数

    Table  1  Chemical and optical parameters for studied samples

    Samples no.Coal mineProximate analysis w/%Ro, max /%Ultimate analysis wdaf/%
    MadAadVdafCHO*NS
    DP-4Dongpo1.5014.2740.350.57377.894.3913.511.162.86
    ML-8Malan0.489.0027.961.20586.324.046.761.111.66
    XM-3Ximing0.708.1815.181.83890.433.733.951.080.72
    *: by difference
    下载: 导出CSV

    表  2  煤样的微晶结构参数

    Table  2  Microcrystalline structure parameters of coal

    Sampled002 /nmLc/nmLa /nm
    DP-40.373 21.238 61.011 9
    ML-80.354 61.749 11.232 4
    XM-30.349 51.952 11.419 1
    下载: 导出CSV

    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 sheetMean d/nmGrouping d/nm
    1×10.390.30-0.54
    2×20.600.55-0.74
    3×30.930.75-1.14
    4×41.271.15-1.44
    5×51.601.45-1.74
    6×61.941.75-2.04
    7×72.282.05-2.44
    8×82.612.45-2.84
    下载: 导出CSV
  • [1] MATHEWS J P, SHARMA A. The structural alignment of coal and the analogous case of Argonne Upper Freeport coal[J]. Fuel, 2012, 95: 19-24. doi: 10.1016/j.fuel.2011.12.046
    [2] YANG J, CHENG S, WANG X, ZHANG Z, LIU X R, TANG G H. Quantitative analysis of microstructure of carbon materials by HRTEM[J]. Trans Nonferrous Met Soc China, 2006, 16(S2): S796-S803. https://www.researchgate.net/publication/229378496_Quantitative_analysis_of_microstructure_of_carbon_materials_by_HRTEM
    [3] SHARMA A, KYOTANI T, TOMITZ A. Direct observation of layered structure of coals by a transmission electron microscope[J]. Energy Fuels, 2000, 14(2): 515-516. doi: 10.1021/ef990253h
    [4] SHARMA A, KYOTANI T, TOMITA A. Comparison of structural parameters of PF carbon from XRD and HRTEM techniques[J]. Carbon, 2000, 34(14): 1977-1984. https://www.researchgate.net/profile/Akira_Tomita/publication/244317503_Comparison_of_structural_parameters_of_PF_carbon_from_XRD_and_HRTEM_techniques/links/560b22ef08ae4d86bb14b96c.pdf?inViewer=0&pdfJsDownload=0&origin=publication_detail
    [5] ASO H, MATSUOKA K, SHARMA A, TOMITA A. Evaluation of size of graphene sheet in anthracite by a temperature-programmed oxidation method[J]. Energy Fuels, 2004, 18(5): 1309-1314. doi: 10.1021/ef030176x
    [6] SHARMA A, KYOTANI T, TOMITA A. A new quantitative approach for microsctructural analysis of coal char using HRTEM images[J]. Fuel, 1999, 78(10): 1203-1212. doi: 10.1016/S0016-2361(99)00046-0
    [7] SHIM H-S, HURT R H, YANG N Y C. A methodology for analysis of 002 lattice fringe images and its application to combustion-derived carbons[J]. Carbon, 2000, 38(1): 29-45. doi: 10.1016/S0008-6223(99)00096-2
    [8] SHARMA A, KYOTANI T, TOMITA A. Direct observation of raw coals in lattice fringe mode using high-resolution transmission electron microscopy[J]. Energy Fuels, 2000, 14(6): 1219-1225. doi: 10.1021/ef0000936
    [9] PALOTÁS A B, RAINEY L C, SAROFIM A F, SANDE J B V, CIAMBELLI P. Effect of oxidation on the microstructure themicrostructure of carbon blacks[J]. Energy Fuels, 1996, 10(1): 254-259. doi: 10.1021/ef950168j
    [10] WORNAT M J, HURT R H, YANG N Y C, HEADLEY T J. Structural and compositional transformations of biomass chars during combustion[J]. Combust Flame, 1995, 100(1/2): 131. https://www.researchgate.net/publication/222216211_Structural_and_compositional_transformations_of_biomass_chars_during_combustion
    [11] NIEKERK D V, MATHEWS J P. Molecular representations of Permian-aged vitrinite-rich and inertinite-rich South African coals[J]. Fuel, 2010, 89(1): 73-82. doi: 10.1016/j.fuel.2009.07.020
    [12] YEHLIU K, VANDER WAL R L, BOEHMAN A L. Development of an HRTEM image analysis method to quantify carbon nanostructure[J]. Combust Flame, 2011, 158(1): 1837-1851. https://www.researchgate.net/publication/251554845_Development_of_an_HRTEM_image_analysis_method_to_quantify_carbon_nanostructure
    [13] MATHEWS J P, FERNANDEZ-ALSO V, DANIEL J A, SCHOBERT H H. Determining the molecular weight distribution of Pocahontas No. 3 low-volatile bituminous coal utilizing HRTEM and laser desorption ionization mass spectra data[J]. Fuel, 2010, 89(7): 1461-1469. doi: 10.1016/j.fuel.2009.10.014
    [14] CASTRO-MARCANO F, LOBODIN V V, RODGERS R P, MCKENNA A M, MARSHALL A G, MATHEWS J P. A molecular model for Illinois No. 6 Argonne Premium coal: Moving toward capturing the continuum structure[J]. Fuel, 2012, 95: 35-49. doi: 10.1016/j.fuel.2011.12.026
    [15] 郭亚楠, 唐跃刚, 王绍清, 李薇薇, 贾龙.树皮残植煤显微组分分离及高分辨透射电镜图像分子结构[J].煤炭学报, 2013, 38(6): 1019-1024. http://www.cnki.com.cn/Article/CJFDTOTAL-MTXB201306023.htm

    GUO Ya-nan, TANG Yue-gang, WANG Shao-qing, LI Wei-wei, JIA Long. Maceral separation of bark liptobiolite and molecular structure study through high resolution TEM images[J]. J China Coal Soc, 2013, 38(6): 1019-1024. http://www.cnki.com.cn/Article/CJFDTOTAL-MTXB201306023.htm
    [16] CASTRO-MARCANO F, LOBODIN V V, RODGERS R P, MCKENNA A M, MARSHALL A G, MATHEWS J P. A molecular model for Illinois No. 6 Argonne Premium coal: Moving toward capturing the continuum structure[J]. Fuel, 2012, 95: 35-49. doi: 10.1016/j.fuel.2011.12.026
    [17] 任秀彬, 辛文辉, 张亚婷, 周安宁.基于HRTEM的低阶烟煤微晶结构研究[J].煤炭学报, 2015, 40(S1): 242-246. http://www.cnki.com.cn/Article/CJFDTOTAL-MTXB2015S1037.htm

    REN Xiu-bin, XIN Wen-hui, ZHANG Ya-ting, ZHOU An-ning. Structural alignment of low rank coal using HRTEM technique[J]. J China Coal Soc, 2015, 40(S1): 242-246. http://www.cnki.com.cn/Article/CJFDTOTAL-MTXB2015S1037.htm
    [18] 张小东, 孔令菲, 秦勇, 张鹏.龙口褐煤萃取后微晶结构的XRD与HRTEM研究[J].煤炭学报, 2013, 38(6): 1025-1030. http://www.cnki.com.cn/Article/CJFDTOTAL-MTXB201306024.htm

    ZHANG Xiao-dong, KONG Ling-fei, QIN Yong, ZHANG Peng. Research on the microcrystalline structure of the fractionally-extracted Longkou lignite by XRD and HRTEM[J]. J China Coal Soc, 2013, 38(6): 1025-1030. http://www.cnki.com.cn/Article/CJFDTOTAL-MTXB201306024.htm
    [19] JU Y W, LI X S. New research progress on the ultrastructure of tectonically deformed coals[J]. Prog Nat Sci, 2009, 19(11): 1455-1466. doi: 10.1016/j.pnsc.2009.03.013
    [20] ENDO M, FURUTA T, MINOURA F, KIM C, OSHIDA K, DRESSELHAUS G, DRESSELHAUS M S. Visualized observation of pores in activated carbon fibers by HRTEM and combined image processor[J]. Supramol Sci, 1998, 5(S3/4): 261-266. https://www.researchgate.net/publication/222946259_Visualized_observation_of_pores_in_activated_carbon_fibers_by_HRTEM_and_combined_image_processor
    [21] TAKAGI H, MARUYAMA K, YOSHIZAWA N, YAMAD A Y, SATO Y. XRD analysis of carbon stacking structure in coal during heat treatment[J]. Fuel, 2004, 83(S17/18): 2427-2433. https://www.researchgate.net/publication/223675644_XRD_analysis_of_carbon_stacking_structure_in_coal_during_heat_treatment
    [22] HUANG Z H, KANG F Y, HUANG W L, YANG J B, LIANG K M, CUI M L, CHENG Z Y. Pore structure and fractal characteristics of activated carbon fibers characterized by using HRTEM[J]. J Colloid Interface Sci, 2002, 249(2): 453-457. doi: 10.1006/jcis.2002.8274
    [23] PALOTAS A B, RAINEY L C, FELDERMANN C J, SAROFIM A F, Vander SANDE J B. Soot morphology: An application of image analysis in high-resolution transmission electron microscopy[J]. Microsc Res Technol, 1996, 33(3): 266-278. doi: 10.1002/(ISSN)1097-0029
    [24] 杨起.中国煤变质作用[M].北京:煤炭工业出版社, 1996: 154.

    YANG Qi. The Coal Metamorphism in China[M]. Beijing: Press of Coal Industry, 1996: 154.
    [25] 赵峰华, 任德贻.应用高分辨率透射电镜研究煤显微组分的结构[J].地质论评, 1995, 41(6): 564-570. http://www.cnki.com.cn/Article/CJFDTOTAL-DZLP199506011.htm

    ZHAO Feng-hua, REN De-yi. The application of high-resolution transmission electron microscopy to study the structures of coal macerals[J]. Geol Rev, 1995, 41(6): 564-570. http://www.cnki.com.cn/Article/CJFDTOTAL-DZLP199506011.htm
    [26] CABIOC'H T, THUNE E, JAOUEN M. Carbon-onion thin-film synthesis onto silica substrates[J]. Chem Phys Lett, 2000, 320(1/2): 202-205. https://www.researchgate.net/publication/235126829_Carbon-onion_thin-film_synthesis_onto_silica_substrates
    [27] 韩德馨.中国煤岩学[M].徐州:中国矿业大学出版社, 1996: 260.

    HAN De-xin. Coal Petrology in China[M]. Xuzhou: China University of Mining and Technology Press, 1996: 260.
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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

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