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1 PETROLEUM EXPLORATION AND DEVELOPMENT Vol.43 No.3 文章编号 : (2016) DOI: /PED 微纳米孔隙空间三维表征与连通性定量分析孙亮 1, 2, 王晓琦 1, 2, 金旭 1, 2, 李建明 1, 2, 吴松涛 1, 2 (1. 国家能源致密油气研发中心 ;2. 中国石油勘探开发研究院 ) 基金项目 : 国家重点基础研究发展计划 (973) 项目 (2014CB239000); 国家科技重大专项 (2011ZX05001) 摘要 : 利用 FIB-SEM( 聚焦电子 - 离子双束扫描电镜 ) 三维成像表征技术和数字岩石技术, 开展非常规储集层孔隙连通性评价研究利用 FIB-SEM 三维成像功能得到高分辨率的储集层数字图像, 通过形状矫正亮度矫正景深矫正和物相区分等数字岩石技术将数字图像转换为可供进一步分析的孔隙结构数字模型, 基于此模型提出一种孔隙连通性评价方法, 将孔隙连通域进行分级 : 死连通域为孤立孔隙,1 级连通域最差,3 级连通域最好 ; 在此基础上统计各级连通率并进行连通域提取, 对特定连通域进行数量体积和形状等参数的统计分析, 从而实现孔隙空间的量化表征实例应用表明纳米合成材料页岩致密碳酸盐岩连通率具有显著差异 ( 分别为 96% 22% 和 82%), 连通域数量体积和形状分布规律亦不同 ; 通过上述量化指标 ( 各级连通率连通域数量体积和形状参数 ), 有效区分了此 3 类典型材料和储集层的孔隙空间特征, 证实了该方法的有效性图 12 表 2 参 13 关键词 : 微纳米孔隙 ; 孔隙结构 ; 孔隙连通性 ; 非常规油气 ; 四川盆地 ; 准噶尔盆地中图分类号 :TE122 文献标识码 :A Three dimensional characterization and quantitative connectivity analysis of micro/nano pore space SUN Liang 1, 2, WANG Xiaoqi 1, 2, JIN Xu 1, 2, LI Jianming 1, 2, WU Songtao 1, 2 (1. National R&D Center of Tight Oil & Gas, Beijing , China; 2. PetroChina Research Institute of Petroleum Exploration & Development, Beijing , China) Abstract: Evaluation is performed on pore connectivity of unconventional reservoirs using 3-D FIB-SEM imaging characterization and digital rock techniques. 3-D images are first obtained by FIB-SEM device and then transformed into digital pore structure model through shape correction, brightness correction, depth-of-field correction and phase distinguishing. Based on this model, a new connectivity evaluation method for micro/nano pores in unconventional reservoirs is proposed. This method differentiates dead and live pore space, grades live connected domains (1-grade is the worst and 3-grade is the best) and calculates the connectivity rates of all grades. Selected connected domains can be quantitatively characterized through statistical analysis of connected domain distribution, volume and shape. The applications on nano material, shale and carbonate get distinctive connectivity rates (96%, 22% and 82%) and characteristic differences on connected domain distribution, volume and shape. Through these statistical parameters (connectivity rate, connected domain distribution, volume and shape), the three demonstrated materials and reservoirs are quantitatively characterized and differentiated. Thus, validity of the proposed connectivity method in this paper is proved. Key words: micro/nano pore space; pore structure; pore connectivity; unconventional hydrocarbon; Sichuan Basin; Junggar Basin 0 [1-5] 1 CT - FIB-SEM 2

2 [4] [6] [7-8] 图 1 FIB-SEM 三维成像样品准备工作示意图 [9-10] FIB-SEM 三维成像 Focused Ion Beam FIB 图 2 电子束离子束和样品角度关系示意图 Scanning Electron Microscope SEM 3 3 FIB SEM 10~20 μm FIB 2 4 FEI Helios NanoLab 650 FIB-SEM 2 1 kv 0.9 nm 5 6~20 h 1 FIB-SEM 1.2 基于 FIB-SEM 的三维数字岩石技术及关键问题 FIB-SEM CT FIB-SEM FIB-SEM FIB-SEM

3 492 Vol. 43 No.3 FIB-SEM 图像尺度与位置矫正 SEM FIB-SEM 3 Helios 52 FIB-SEM SEM y 2 sin52 FIB-SEM y x z y FIB-SEM CT y Avizo Correct Z Drop y FIB-SEM FIB-SEM y z z Correct Z Drop a exp b u a b u a b a=1 b 0 1 Avizo FIB-SEM b FIB Wizard [11-12] FIB-SEM Align Slices 景深与物相分割 FIB-SEM SEM SEM 亮度矫正 FIB-SEM

4 Avizo [12] Histogram Histogram 2D-Histogram [12] 图 3 种子填充法示意图连通域检测 2.2 连通域分级 [13] [13]

5 494 Vol. 43 No.3 FIB-SEM 图 4 连通性分级 V / V 1 p V V 2 e ep / 纳米合成材料孔隙连通性评价 Cr Vep / Vp 3 FIB-SEM 6a x y z Cr Cr1+ Cr2+ Cr nm 8.03 nm Cr1= V / Vp nm Cr2= V / Vp 6 x Cr3= V / Vp 7 y z 连通域提取 6b Avizo FIB Align Wizard Correct Z Drop FIB-SEM D-Histogram [12] 6c 3 Matlab 图 5 连通域提取

6 图 6 纳米合成材料三维成像及孔隙模型 % 图 7 纳米合成材料 FIB-SEM 三维成像的灰度分布图图 8 纳米合成材料连通域数量分布直方图图 9 纳米合成材料连通域累计体积分布直方图

7 496 Vol. 43 No % 2.8% % 15.91% nm nm 表 1 纳米合成材料的连通性分析 /% 3 / Cr 1 Cr 2 Cr 3 Cr /% ~0.5 60~110 nm 20~30 图 10 连通域表面积与体积之比与体积的关系图 3.2 页岩及致密碳酸盐岩孔隙连通性评价 11 图 11 四川盆地下志留统龙马溪组页岩以及准噶尔盆地二叠系芦草沟组致密碳酸盐岩 FIB-SEM 三维成像 12 2 x y z nm 8.09 nm nm 1.41% 26

8 图 12 四川盆地龙马溪组页岩及准噶尔盆地芦草沟组致密碳酸盐岩连通域数量和连通域累计体积分布直方图表 2 四川盆地龙马溪组页岩及准噶尔盆地芦草沟组致密碳酸盐岩连通性分析 / % / /% Cr 1 Cr 2 Cr 3 Cr 3 /% a 10~ 500 nm % 3.17% 2 20~50 nm 22% 0.3% x y z nm nm nm 3.91% c 1~2 4 1

9 498 Vol. 43 No.3 2 % V m 3 V p m 3 V ep m 3 V p1 V p2 V p m 3 % e % 参考文献 : [1] LOUCKS R G, REED R M, RUPPEL S C, et al. Morphology, genesis, and distribution of nanometer-scale pores in siliceous mudstones of the Mississippian Barnett Shale[J]. Journal of Sedimentary Research, 2009, 79(12): [2] SLATT R M, O'BRIEN N R. Pore types in the Barnett and Woodford 3 gas shales: Contribution to understanding gas storage and migration pathways in fine-grained rocks[j]. AAPG Bulletin, 2011, 95(12): [3] ZOU C N. Unconventional petroleum geology[m]. Amsterdam: Elsevier, [4],,,. [J]., 2012, 39(1): ZOU Caineng, YANG Zhi, TAO Shizhen, et al. Nano-hydrocarbon and the accumulation in coexisting source and reservoir[j]. Petroleum Exploration and Development, 2012, 39(1): [5],,,. 5 [J]., 2013, 15(5): ZHU Rukai, BAI Bin, CUI Jingwei, et al. Research advances of microstructure in unconventional tight oil and gas reservoirs[j]. Journal of Palaeogeography, 2013, 15(5): [6] VOGEL H. Morphological determination of pore connectivity as a function of pore size using serial sections[j]. European Journal of Soil Science, 1997, 48(3): [7],,. [J]., 2013, 35(6): HUANG Chuanqing, ZHANG Jingong, MA Rui. Analysis on pore structure characteristics and connectivity of mud rocks[j]. Underground Water, 2013, 35(6): [8],,. [J]., 2013, 33(1): YANG Baohua, WU Aixiang, LIU Jinzhi. Analysis of pore connectivity of granular ore media after heap leaching based on digital image processing[j]. Mining and Metallurgical Engineering, 2013, 33(1): [9]. [J]., 2012, 38(19): QI Linhai. Present situation and development trend of digital core technology[j]. Inner Mongolia Petrochemical Industry, 2012, 38(19): [10],,. [J]., 2013, 28(6): LIU Xuefeng, ZHANG Weiwei, SUN Jianmeng. Methods of constructing 3-D digital cores: A review[j]. Progress in Geophysics, FIB-SEM , 28(6): FIB-SEM CT [11] FEI VISUALIZATION SCIENCES GROUP. Learn more about FEI s 3D visualization solutions[db/ol]. ( )[ ]. [12] FEI VISUALIZATION SCIENCES GROUP. Avizo 8.0 user s guide [DB/OL]. ( )[ ]. avizo-3d-user-guide.pdf. [13] HECKBERT P S. A seed fill algorithm[m]//glassner A S, KAUFMANN M. Graphics Gems. California: San Diego, 1990: FEI 符号注释 : Cr % Cr 1 Cr 2 Cr 第一作者简介 : 孙亮 (1983-), 男, 辽宁营口人, 博士, 现为中国石油勘探开发研究院工程师, 主要从事油气储集层表征与非常规油气方面研究地址 : 北京市海淀区学院路 20 号, 中国石油勘探开发研究院石油地质实验研究中心, 邮政编码 : sunliang0315@163.com 收稿日期 : 修回日期 : 魏玮王大锐

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