Multi−scale characterization of shale pore structure of Niutitang Formation in southeastern Guizhou and its influence on shale gas enrichment
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摘要:
研究目的 研究黔东南地区牛蹄塘组页岩孔隙结构特征及其对页岩气富集的影响，抛开不利因素，为黔东南地区页岩气勘探提供建议。
研究方法 通过聚焦离子束扫描电镜（FIB−SEM）、场发射扫描电镜（FE−SEM）和氮气吸附等手段，对页岩微纳米孔隙结构进行多尺度表征，并结合研究区牛蹄塘组页岩的生烃及埋藏史，研究构造运动与孔隙结构关系，进而分析对页岩气富集的影响。
研究结果 牛蹄塘组页岩主要发育毫米级微裂缝、微米级黄铁矿晶间孔以及纳米级有机质孔隙，以墨水瓶状孔隙和平板结构的狭缝孔为主，孔隙结构复杂；结合FIB−SEM三维重构结果，有机质在页岩中占比较高，其孔隙度在0.04%~2.48%，对总孔隙的贡献率介于14%~96%，与有机质共生的黄铁矿晶间孔是沟通裂缝的主要孔隙类型；该地区页岩气赋存状态以欠饱和的吸附气为主，游离气含量偏低。
结论 牛蹄塘组页岩大量构造裂缝，沟通了有机质孔及黄铁矿晶间孔，改变了原有孔隙结构，致使原位聚集的页岩气沿裂缝逸散，是牛蹄塘组页岩含气量低的关键因素。热演化程度适中、构造保存好的区域是古隆起周缘下一步页岩气勘探的有利方向。
Abstract:This paper is the result of oil and gas exploration engineering.
Objective It is necessary to study the pore structure characteristics of Niutitang Formation shale in Southeast Guizhou and its influence on shale gas enrichment, avoid unfavorable factors, and provide suggestions for shale gas exploration in Southeast Guizhou.
Methods Multi−scale characterization of the shale micro−nano pore structure is carried out by means of focused ion beam scanning electron microscopy (FIB−SEM), FE−SEM, and nitrogen adsorption. Combined with the hydrocarbon generation and burial history of the Niutitang Formation shale in the study area, the relationship between tectonic movement and pore structure is studied, and its control effect on shale gas enrichment is analyzed.
Results The Niutitang Formation shale mainly develops millimeter−scale micro−cracks, micron−scale pyrite intercrystalline pores and nano−scale organic pores, mainly ink bottle−shaped pores and slit pores with a flat plate structure, and the pore structure is complex. Combined with the results of FIB−SEM three−dimensional reconstruction, organic matter accounts for a relatively high proportion of shale, with a porosity of 0.04%−2.48% and a contribution rate of 14%−96% to the total porosity. The pyrite crystals co−existing with organic matter Pores are the main type of pores that communicate fractures, the shale gas in this area is dominated by undersaturated adsorbed gas, and the free gas content is low.
Conclusions A large number of structural fractures in the Niutitang Formation shale have connected organic matter pores and pyrite intercrystalline pores, and changed the original pore structure, causing the in−situ accumulated shale gas to escape along the fractures, which is a key factor in the low gas content of the shale of the Niutitang Formation. Finding areas with moderate thermal evolution and well−preserved structures is a favorable direction for shale gas exploration on the periphery of paleo−uplifts.
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图 12 不同尺度下页岩气流动及产出(据Javadpour, 2007)
Figure 12.
表 1 常见的微观孔隙检测方法
Table 1. Common microscopic pore detection methods
检测方法 特点 局限性 氩离子抛光－扫描
电镜/Ar−ion Milling SEM页岩二维孔隙结构的定性研究，能够快速观测页岩样品中的孔隙含量、分布及孔径范围 仅适用于二维微纳米孔隙刻画，无法反映三维空间结构 宽离子束－扫描电镜/ BIB−SEM 场发射扫描电镜/ FE−SEM 页岩二维孔隙结构的定性研究，进行样品表层的微区点线面元素的定性、半定量及定量分析 氦离子扫描电镜/HIM 是FE−SEM的补充，提供更强的样品表面信息对比度机制 小角X射线散射/ SAXS 几十纳米以下微孔隙 后期数据分析处理受限 （超）小角度中子散射/（U）SANS 纳米孔隙分布和几何形态 核磁共振 微纳米孔隙全孔径分析，定性划分有机、无机孔 孔径分布准确性受影响 高压压汞法 微纳米孔隙孔径分布、孔吼形态及发育情况，定性判断孔吼连通性 不适于表征微孔，且造成样品无法二次利用 微米Ｘ射线显微镜/ Micro−CT 表征页岩三维空间结构特征 仅适合于表征页岩亚微米级至微米级孔隙结构 纳米透射Ｘ射线显微镜/Nano−CT 反映三维空间结构，更加精确地实现页岩组分定量研究 分辨率有限，不适宜表征页岩介孔及微孔 聚焦离子束−扫描电镜/FIB−SEM 数纳米级分辨率下，对页岩孔隙进行三维重构，定性、定量分析纳米—微米级孔隙度、孔径及连通性 页岩纳米级孔隙三维结构研究的主要技术手段，视域小，需结合MAPS技术综合分析 
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表 2 样品基本信息
Table 2. Basic information of samples
序号 层段 岩性 TOC/% Ro/% 石英/% 碳酸盐/% 黄铁矿/% 伊利石相对含量/% HD−1 牛蹄塘组上段 含碳酸盐钙质页岩 2.5 1.44 28 35 3 37 HD−2 牛蹄塘组上段 含碳质页岩 1.39 2.12 35 4 4 32 HD−3 牛蹄塘组上段 含碳质页岩 0.84 2.65 34 0 4 34 HD−4 牛蹄塘组上段 含碳质页岩 2 / 29 9 4 27 HD−5 牛蹄塘组中段 含粉砂质碳质页岩 0.79 / 32 / 4 39 HD−6 牛蹄塘组中段 含粉砂质碳质页岩 5.85 2.71 28 4 11 43 HD−7 牛蹄塘组下段 碳质页岩 5.67 / 43 7 6 40 HD−8 牛蹄塘组下段 碳质页岩 2.97 / 43 4 6 45 HD−9 牛蹄塘组下段 含粉砂质碳质页岩 3 2.79 43 4 5 45 HD−10 牛蹄塘组下段 碳质页岩 6.01 / 53 5 4 48
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表 3 黄地1井页岩样品三维重构结果
Table 3. 3D reconstruction results of shale samples in Huangdi Well 1
样品编号 深度/m 三维重构孔隙度/% 有机质孔隙度/% 贡献率/% 孔径分布区间/nm 有机质占比重/% 黄铁矿占比重/% HD−1 1285.40 0.42 / / 10~60 7.77 2.68 HD−2 1292.30 0.37 0.08 22.29 10~100 3.18 2.91 HD−3 1302.00 0.29 0.04 13.79 10~100 3.63 1.64 HD−6 1331.45 0.58 0.24 41.03 10~100 10.20 4.87 HD−9 1369.95 2.57 2.48 96.56 10~80 21.70 /
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表 4 黄地1井低温N2吸附孔隙结构参数
Table 4. Pore structure parameters of low temperature N2 adsorption in Huangdi Well 1
样品编号 BET比表面积/
(m2/g)BJH 解吸总孔体积/
(mL/g)平均孔径/
nmHD−1 4.273 0.00123 3.3 HD−2 3.933 0.00118 3.13 HD−3 6.693 0.00411 3.86 HD−4 6.692 0.00788 5.64 HD−5 7.035 0.00335 3.45 HD−6 10.023 0.00438 3.2 HD−7 13.411 0.00101 2.37 HD−8 8.091 0.00398 3.31 HD−9 5.178 0.00103 3.05 HD−10 11.248 0.00319 2.68
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