Pore Structure Characteristics and Comparisons of Upper Permian Longtan and Dalong Formation Transitional Facies Shale in Xiangzhong-Lianyuan Depression
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摘要: 以湘中坳陷涟源凹陷上二叠统龙潭组和大隆组海陆过渡相泥页岩为研究对象，重点选取12块典型泥页岩钻井岩心样品开展有机碳含量、岩石热解、X射线衍射、密度法孔隙度、高压压汞、二氧化碳和氮气吸附等测试分析，利用氩离子抛光-场发射扫描电镜（FE-SEM）观察了泥页岩孔隙特征，通过定性描述和定量测定相结合的方法研究了海陆过渡相泥页岩纳-微米级孔隙结构特征及孔隙发育影响因素.研究结果表明：龙潭组和大隆组泥页岩有机碳含量均较高，热演化程度处在凝析油和湿气生成阶段早期，对应Ro为1.22%~1.43%；泥页岩孔隙类型主要为粒间孔、粒内孔、有机孔和微纳米缝.龙潭组与大隆组样品在孔隙形态、孔隙大小和影响因素上均有差异：龙潭组样品氮气吸附滞回环开口宽，有机孔形态多为圆形和椭圆形，孔径较大；大隆组样品氮气吸附滞回环开口窄，有机孔形态多为不规则状，孔径较小；龙潭组泥岩和大隆组泥页岩样品有机碳含量与黏土矿物含量呈正相关关系，2套样品的微孔孔隙积体与有机碳和黏土矿物含量均呈正相关性；龙潭组样品介孔+宏孔的孔隙体积与有机碳和黏土矿物含量呈正相关性，与石英+长石含量呈负相关性；大隆组样品中的碳酸盐矿物对其孔隙性有明显影响，大隆组样品介孔+宏孔孔隙体积与有机碳、黏土矿物和石英+长石含量相关性不明显.Abstract: Taking transitional facies shale of Permian Longtan and Dalong Formations as the research object, 12 typical drilling core shale samples in Xiangzhong-Lianyuan depression were selected for tests including organic carbon content, rock-eval, X-ray diffraction, density porosity, high-pressure mercury intrusion, CO2/N2 adsorption while using field emission scanning electron microscopy(FE-SEM) to observe pore characteristics. In this study it focuses on the development of nano-microscale pore, pore structure characteristics and main control factors of the transitional facies shale through the combinations of qualitative description and quantitative measure method. The results show that the organic carbon content of Longtan and Dalong Formation shales is high, the degree of thermal evolution is in the early stage of generating condensate oil and wet gas, corresponding to Ro of 1.22%-1.43%; pore types of shale are mainly intergranular pores, intragranular pores, organic pores and micro-nanoscale cracks. There are differences in the pore morphology, pore size and control factors between Longtan and Dalong Formations. In Longtan Formation, N2 adsorption hysteresis loop is wide and the shapes of organic poresare mostly round and elliptic with larger pore diameter. The N2 adsorption hysteresis loop of the Dalong Formation is narrow and the shapes of the organic poresare irregular with small pore diameter. There is a positive correlation between TOC and clay mineral in both Longtan and Dalong Formation shales. The volume of micropore in both Longtan and Dalong Formation shales is positively correlated with TOC and clay mineral. The mesopore+macropore pore volume of Longtan Formation shale has a position linear relationship with TOC and clay mineral, but is negatively correlated with quartz+feldspar. Carbonate mineral in Dalong Formation has a significant influence on its pore structure, and the relationship of mesopore+macropore pore volume with TOC-clay mineral and quartz+feldspar in Dalong Formation shale is not obvious.
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图 1 湘中坳陷区域构造位置(a)、涟源凹陷构造分区(b)和涟源凹陷CD构造剖面
Fig. 1. Sketch of the regional structure location of Xiangzhong depression (a), structural zoning map of Lianyuan depression (b) and CD tectonic profile of Lianyuan depression
图 2 涟源凹陷XY1井上二叠统综合柱状图及岩心样品相关信息
Fig. 2. Integrated column of Upper Permian in Well XY1 in Lianyuan depression and core sample information
图 3 涟源凹陷XY1井龙潭组和大隆组样品矿物组成特征
Fig. 3. Mineral composition characteristics of Longtan and Dalong Formation shales of Well XY1 in Lianyuan depression
图 4 龙潭组和大隆组样品无机孔和微纳米裂缝形态及发育特征的FE-SEM图像照片
a.方解石和白云石颗粒中和颗粒边缘发育的溶蚀孔、粒间孔，XY1井600.22 m，大隆组; b.黄铁矿中的有机孔和黏土矿物层间孔隙，XY1井600.22 m，大隆组; c.方解石颗粒内溶蚀孔，XY1井600.22 m，大隆组; d.金红石颗粒中发育的粒内孔，XY1井600.22 m，大隆组; e.草莓状黄铁矿颗粒之间的粒间孔，左侧可见粒间孔，XY1井624.87 m，大隆组; f.矿物颗粒边缘发育大量三角形粒间孔，也可见黏土矿物与矿物颗粒间孔隙，XY1井600.22 m，大隆组; g.絮状伊利石层间孔隙，XY1井692.66 m，龙潭组; h.高岭石层间孔隙，XY1井692.66 m，龙潭组; i.黏土矿物与有机质复合体，XY1井692.66 m，龙潭组; j.方解石颗粒内部构造微纳米缝，XY1井600.22 m，大隆组; k.构造微纳米缝，XY1井692.66 m，龙潭组; l.成岩收缩微纳米缝，XY1井692.66 m，龙潭组
Fig. 4. Morphology and development characteristics of FE-SEM pictures of non-organic pores and micro-nano cracks of the shale samples in Longtan and Dalong Formations
图 5 龙潭组和大隆组样品有机孔形态及发育特征的FE-SEM图像照片
a.有机质颗粒内发育不规则状有机孔，红色充填，XY1井624.87 m，TOC=5.07%，大隆组; b.有机质颗粒内发育的不规则状有机孔，红色充填，XY1井624.87 m，TOC=5.07%，大隆组; c.充填在黄铁矿晶体间的有机质，发育有大量的椭圆状、不规则状有机孔，大孔内可见小孔，红色充填，XY1井600.22 m，TOC=3.69%，大隆组; d.长条状有机质颗粒内发育不规则状有机孔，红色充填，XY1井624.87 m，TOC=5.07%，大隆组; e.有机质颗粒内发育不规则状有机孔，红色充填，XY1井624.87 m，TOC=5.07%，大隆组; f.有机质颗粒内发育的椭圆形-近圆形有机孔，红色充填，XY1井692.66 m，TOC=10.29%，龙潭组; g.长条状有机质颗粒内发育的椭圆形-近圆形有机孔，红色充填，可见不发育有机孔的长条状致密有机质颗粒，XY1井692.66 m，TOC=10.29%，龙潭组; h.有机质颗粒内发育的椭圆形-近圆形有机孔，红色充填，XY1井692.66 m，TOC=10.29%，龙潭组; i.有机质颗粒内发育椭圆形有机孔，红色充填，XY1井692.66 m，TOC=10.29%，龙潭组
Fig. 5. Morphology and development characteristics FE-SEM pictures of organic pores of the shale samples in Longtan and Dalong Formations
图 6 龙潭组和大隆组样品CO2吸附曲线和N2吸附-脱附曲线
Fig. 6. CO2 adsorption isotherms and N2 adsorption-desorption isotherms of the shale samples in Longtan and Dalong Formations
图 7 龙潭组和大隆组样品CO2和N2气体吸附测试获得的孔径分布
Fig. 7. Pore size distribution by CO2 and N2 adsorption of the shale samples in Longtan and Dalong Formations
图 8 龙潭组和大隆组泥页岩样品高压压汞进-退汞曲线
Fig. 8. Injection-withdrawal curves of the shale in Longtan and Dalong Formations based on the high pressure mercury intrusion method
图 9 龙潭组和大隆组泥页岩样品不同孔喉直径范围的孔隙体积占比直方图
Fig. 9. Pore volume proportion histograms within different pore diameter ranges of the shale samples in Longtan and Dalong Formations
图 10 龙潭组和大隆组样品TOC与黏土矿物和孔隙体积与TOC以及矿物组成关系
Fig. 10. Correlation between TOC and clay mineral, pore volume and TOC, pore volume and mineral compositions of Longtan and Dalong Formation shale samples
表 1 涟源凹陷XY1井龙潭组和大隆组样品的有机碳测定数据
Table 1. Total organic carbon (TOC) contents of Longtan and Dalong Formation samples of Well XY1 in Lianyuan depression
层位 小层 岩性 深度范围（m） 厚度（m） TOC范围（%） TOC均值（%） 大隆组 ③ 灰色灰质泥页岩夹页岩 561~592 31 0.69~4.69 2.19（12） ② 深灰色灰质泥页岩夹页岩 592~642 50 1.52~6.79 3.87（21） ① 灰色泥灰岩夹页岩 642~677 35 1.02~4.10 2.00（12） ② 灰色粉砂质泥岩和泥质粉砂岩 677~687 10 1.72~2.10 1.91（2） 龙潭组 ① 黑色碳质泥岩和深灰色泥岩 687~701 14 4.88~10.29 7.45（3） 其中夹薄煤层（劣煤） 694.5~696.5 2 38.41（1） / 注：（）内为有机碳测定的样品数. 
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表 2 龙潭组和大隆组12块样品的有机地化测试数据
Table 2. Organic geochemistry data of 12 samples in Longtan and Dalong Formations
样品编号 层位 岩性 井深（m） 有机碳（TOC，%） 热解峰温（Tmax, ℃） 生烃潜力（S1+S2, mg/g） 镜质体反射率（%） XGY-1 大隆组 灰质泥页岩 600.22 3.69 460 2.66 1.34 XGY-2 大隆组 602.67 2.72 / / / XGY-3 大隆组 608.08 4.96 / / 1.22 XGY-4 大隆组 612.76 5.09 458 4.02 1.37 XGY-5 大隆组 624.87 5.07 448 3.90 / XGY-6 大隆组 629.59 3.13 / / / XGY-7 大隆组 631.18 6.79 451 4.91 / XGY-8 大隆组 641.78 3.00 461 2.66 1.27 XGY-9 龙潭组 粉砂质泥岩 685.07 1.72 / / / XGY-10 龙潭组 泥岩 689.10 7.17 / / / XGY-11 龙潭组 碳质泥岩 692.66 10.29 469 6.00 1.41 XGY-12 龙潭组 劣煤 697.81 38.41 472 36.90 1.43
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表 3 龙潭组和大隆组12块样品矿物组成数据
Table 3. Mineral composition data of 12 samples in Longtan and Dalong Formations
样品编号 层位 全岩定量分析（%） 黏土矿物相对含量（%） 石英 长石 铁白云石 方解石 黏土矿物 黄铁矿 菱铁矿 伊利石 伊蒙混层 高岭石 XGY-1 大隆组 60 6 2 10 20 2 / 4 96 / XGY-2 大隆组 63 3 2 23 8 1 / 7 93 / XGY-3 大隆组 45 7 4 19 23 2 / 5 95 / XGY-4 大隆组 49 7 1 22 18 3 / 30 70 / XGY-5 大隆组 33 7 2 19 36 3 / 17 83 / XGY-6 大隆组 55 4 6 20 13 2 / 16 84 / XGY-7 大隆组 49 5 / 10 33 3 / 2 98 / XGY-8 大隆组 29 8 / 38 21 4 / 19 81 / XGY-9 龙潭组 53 16 / / 31 / / 7 88 5 XGY-10 龙潭组 14 5 / 2 57 / 22 6 68 26 XGY-11 龙潭组 32 3 5 / 60 / / 5 80 15 XGY-12 龙潭组劣煤 40 / / / 48 12 / 7 46 47
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表 4 龙潭组和大隆组样品有机孔形状参数及有机质面孔率统计表
Table 4. Statistics of organic pore shape parameters and surface porosity of the samples in Longtan and Dalong Formations
层位 等效圆孔径平均值（nm） 最小孔径平均值（nm） 最大孔径平均值（nm） 有机孔发育平均数/μm2（个） 单颗粒有机质面孔率范围(%) 有机质面孔率平均值(%) 大隆组 33.73 28.80 50.41 50 4.27~8.05 5.84 龙潭组 254.85 206.58 271.78 2 3.29~14.49 7.26
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表 5 龙潭组和大隆组样品真密度、密度法孔隙度、CO2和N2气体吸附测试的比表面积和孔隙体积数据
Table 5. True density, density porosity, specific surface area and pore volume by N2 and CO2 adsorption analysis of the shale sam- ples in Longtan and Dalong Formations
样品编号 层位 TOC
（%）真密度
（cm3·g-1）密度法孔隙度
（%）总比表面积
（m2·g-1）总孔隙体积
（cm3·g-1）微孔比表面积
（m2·g-1）微孔体积
（cm3·g-1）介孔比表面积
（m2·g-1）介孔体积
（cm3·g-1）宏孔比表面积
（m2·g-1）宏孔体积
（cm3·g-1）XGY-1 大隆组 3.69 2.618 2.0 12.344 0.011 11.151 0.004 1.062 0.003 0.131 0.004 XGY-2 大隆组 2.72 2.618 5.3 11.046 0.010 7.990 0.003 1.462 0.003 1.593 0.004 XGY-3 大隆组 4.96 2.625 7.4 15.880 0.014 13.107 0.005 2.621 0.004 0.153 0.005 XGY-4 大隆组 5.09 2.650 1.4 12.357 0.014 10.857 0.004 1.277 0.003 0.222 0.007 XGY-5 大隆组 5.07 2.684 5.1 11.233 0.007 10.757 0.003 0.382 0.002 0.094 0.003 XGY-6 大隆组 3.13 2.720 6.0 7.798 0.009 6.568 0.002 1.080 0.003 0.150 0.005 XGY-7 大隆组 6.79 2.580 4.5 13.727 0.011 12.565 0.004 1.028 0.003 0.134 0.004 XGY-8 大隆组 3.00 2.660 2.3 11.698 0.012 9.152 0.003 2.411 0.004 0.135 0.004 XGY-9 龙潭组 1.72 2.726 5.6 13.536 0.017 10.592 0.004 2.720 0.007 0.224 0.007 XGY-10 龙潭组 7.17 2.648 4.9 40.017 0.026 32.868 0.010 6.988 0.012 0.161 0.004 XGY-11 龙潭组 10.29 2.677 12.6 38.254 0.028 30.99 0.009 7.039 0.013 0.225 0.006 XGY-12 龙潭组 38.41 2.304 2.9 34.512 0.016 33.651 0.010 0.721 0.002 0.140 0.004
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