黔北寒武系牛蹄塘组页岩孔隙分形表征

doi:10.13745/j.esf.sf.2022.5.36

地学前缘 ›› 2023, Vol. 30 ›› Issue (3): 110-123.DOI: 10.13745/j.esf.sf.2022.5.36

黔北寒武系牛蹄塘组页岩孔隙分形表征

唐玄¹(), 郑逢赞¹, 梁国栋¹, 马子杰¹^,², 张家政³, 王玉芳³, 张同伟⁴

1.中国地质大学(北京) 自然资源部页岩气资源战略评价重点实验室, 北京 100083
2.贵州省煤层气页岩气工程技术研究中心, 贵州贵阳 550000
3.中国地质调查局油气资源调查中心, 北京 100083
4.Bureau of Economic Geology, Jackson School of Geosciences, The University of Texas at Austin, Austin, TX 78713, USA

收稿日期:2022-02-10 修回日期:2022-04-20 出版日期:2023-05-25 发布日期:2023-04-27
作者简介:唐玄(1979—),男,教授,博士生导师,长期从事页岩油气地质研究与资源评价工作。E-mail: Tangxuan@cugb.edu.cn
基金资助:
国家自然科学基金项目(41730421);国家自然科学基金项目(41972132);中央高校基本科研业务费项目(35832020051)

Fractal characterization of pore structure in Cambrian Niutitang shale in northern Guizhou, southwestern China

TANG Xuan¹(), ZHENG Fengzan¹, LIANG Guodong¹, MA Zijie¹^,², ZHANG Jiazheng³, WANG Yufang³, ZHANG Tongwei⁴

1. MNR Key Laboratory for Strategic Evaluation of Shale Gas Resources, China University of Geosciences (Beijing), Beijing 100083, China
2. Guizhou Engineering Technology Research Center for Goalbed Methane and Shale Gas,Guiyang 550000, China
3. Oil and Gas Resources Survey Center of China Geological Survey, Beijing 100083, China
4. Bureau of Economic Geology, Jackson School of Geosciences, The University of Texas at Austin, Austin, TX 78713, USA

Received:2022-02-10 Revised:2022-04-20 Online:2023-05-25 Published:2023-04-27

摘要/Abstract

摘要：

页岩的孔隙结构是影响页岩气赋存和流动的关键因素,分形维数可以用来定量描述页岩孔隙结构的复杂程度。以黔北地区牛蹄塘组富有机质页岩为例,在扫描电镜、页岩地球化学和矿物组成分析基础上,利用高压压汞和低温氮气吸/脱附法研究了页岩孔隙结构特征参数,利用FHH模型计算了孔隙分形维数,讨论了孔隙结构的影响因素。研究发现:(1)下寒武统牛蹄塘组富有机质页岩石英含量为39.0%~68.4%;黏土矿物含量为11.5%~28.2%;有机碳含量为2.77%~5.81%,平均为3.81%;有机质成熟度高。(2)氮气吸脱附数据显示BET比表面积为11.954~21.744 m²/g,平均为14.572 m²/g;总孔体积为0.018 6~0.025 9 cm³/g,平均为0.021 4 cm³/g;平均孔径范围在4.773~7.025 nm,平均为5.967 nm。微孔对总比表面积贡献大,而中孔和宏孔对孔隙体积贡献大。(3)基于低温氮气吸附数据获得的页岩孔隙分形维数D₁和D₂分布相对集中(D₁为2.65~2.71,D₂为2.79~2.85),压汞数据的大孔隙分形维数分布范围宽(D_Hg为2.21~2.81),分形维数显示牛蹄塘组富有机质页岩具有以微孔为主的复杂孔隙结构和高度非均质性,孔隙发育具有多重分形特征。(4)分形维数D₂与有机碳含量和微孔体积有明显的正相关关系,显示分形维数D₂可用于有机质孔隙结构表征,而矿物组成对分形维数没有明显影响。研究区牛蹄塘组页岩分形维数与龙马溪组产气页岩较为接近,指示本区页岩具有较好的孔隙结构。

关键词: 孔隙结构, 分形维数, 牛蹄塘组, 高压压汞, 黔北地区

Abstract:

Pore structure is the key factor affecting the distribution and flow of shale gas, and fractal analysis can be used to quantitatively characterize the complex pore structures in shale. To better understand the porous structure of the organic-rich shale from the Lower Cambrian Niutitang Formation in northern Guizhou Province, southeastern China, shale samples from Well ZK, Songtao area, are analyzed to determine the pore parameters using high-pressure mercury injection and low-temperature nitrogen adsorption methods, combined with scanning electron microscope observation, shale geochemistry and mineral composition analysis. The pore fractal dimensions are calculated by FHH model, and the influencing factors for pore structure are discussed. To summarize: (1) the quartz content in the organic-rich shale ranges between 39%-68.4%; clay content, 11.5%-28.2%; organic carbon content, 2.77%-5.81% (average 3.81%); while kerogen is mainly of type I, with high thermal maturity. (2) The BET specific surface area ranges between 11.954-21.744 m²/g (average 14.572 m²/g); total pore volume, 0.0186-0.0259 cm³/g (average 0.0214 cm³/g); and average pore size, 4.773-7.025 nm (average 5.967 nm). Micropores contribute largely to the total specific surface area; while mesopores and macropores account for a large proportion of pore volume. (3) The organic-rich shale has complex pore structure dominated by micropores, with high heterogeneity and multifractal characteristics. The pore fractal dimensions D₁ and D₂ obtained from low-temperature nitrogen adsorption data have narrow pore-size distributions (D₁, 2.65-2.71; D₂, 2.79-2.85), while mercury injection data yield a wider pore-size distribution for macropores (D_Hg between 2.21-2.81). (4) D₂ is positively correlated with TOC content and micropore volume, and mineral composition has no significant effect on pore fractal dimensions. The fractal dimension of the Niutitang shale in the study area is similar to that of the gas-producing Longmaxi shale, indicating shales of this area have good pore structure.

Key words: pore structure, fractal dimension, Niutitang Formation, high pressure mercury injection, northern Guizhou Province

中图分类号:

唐玄, 郑逢赞, 梁国栋, 马子杰, 张家政, 王玉芳, 张同伟. 黔北寒武系牛蹄塘组页岩孔隙分形表征[J]. 地学前缘, 2023, 30(3): 110-123.

TANG Xuan, ZHENG Fengzan, LIANG Guodong, MA Zijie, ZHANG Jiazheng, WANG Yufang, ZHANG Tongwei. Fractal characterization of pore structure in Cambrian Niutitang shale in northern Guizhou, southwestern China[J]. Earth Science Frontiers, 2023, 30(3): 110-123.

图/表 15

表1 黔北松桃ZK钻孔下寒武统牛蹄塘组页岩样品有机质相关参数与矿物成分表

Table 1 Organic matter parameters and mineral compositions of the Lower Cambrian Liutitang Formation shale samples from Well ZK in Songtao, northern Guizhou

样品号	深度/m	TOC含量/%	TOS含量/%	有机质元素比		δ¹³C_PDB/‰	矿物组成含量/%
样品号	深度/m	TOC含量/%	TOS含量/%	H/C	O/C	δ¹³C_PDB/‰	石英	钾长石	斜长石	方解石	(铁)白云石	黄铁矿	黏土矿物
ZK1	1 322.40	3.43	4.08	0.16	0.06	-31.6	46.2	4.0	17.0	1.2	2.7	3.8	25.1
ZK2	1 323.85	3.97	3.47	—	—	—	57.0	4.9	12.2	1.2	0	3.3	21.4
ZK 3	1 324.35	3.13	2.95	0.22	0.04	-31.6	45.9	—	16.3	1.1	5.8	3.5	27.4
ZK 4	1 325.58	4.26	3.17	—	—	—	55.7	2.6	15.6	1.4	2.0	6.1	16.6
ZK 5	1 326.37	3.19	2.59	0.11	0.03	-31.2	57.0	—	9.2	—	1.4	2.9	29.5
ZK 6	1 328.45	2.8	2.74	—	—	—	51.3	4.6	10.6	0.8	—	5.9	26.8
ZK 7	1 330.82	3.22	2.77	0.14	0.04	-32.2	59.9	4.3	9.9	2.2	—	3.5	20.2
ZK 8	1 331.65	2.85	2.47	—	—	—	63.9	8.5	11.6	2.0	—	2.5	11.5
ZK 9	1 332.45	2.77	2.04	0.16	0.03	-32.1	57.9	3.9	12.1	1.4	—	2.5	22.2
ZK 10	1 334.38	3.00	2.29	—	—	—	68.4	—	11.0	1.1	—	2.7	16.8
ZK 11	1 336.55	4.19	2.78	0.11	0.03	-31.8	52.5	8.8	11.4	—	1.4	6.1	19.8
ZK 12	1 337.35	5.65	3.33	—	—	—	48.0	9.0	12.9	—	1.4	3.4	25.3
ZK 13	1 338.86	4.53	2.12	0.16	0.03	-32.1	56.3	—	12.9	—	0	2.5	28.3
ZK 14	1 339.03	4.32	2.66	—	—	—	49.4	2.5	14.7	—	3.0	3.4	27.0
ZK 15	1 339.48	5.81	5.40	0.21	0.05	-31.8	39.0	4.1	15.2	0.5	1.9	19.9	19.4

图1 贵州省松桃地区牛蹄塘组页岩矿物组分含量构成

Fig.1 Mineral compositions of shale samples from the Niutitang Formation, Songtao, northern Guizhou

图2 黔北松桃地区牛蹄塘组页岩总有机碳与总硫含量(a)及有机元素构成(b) 图b中Ⅰ~Ⅳ指干酪根类型Ⅰ到Ⅳ型。

Fig.2 (a) Plot of TOC vs. TOS contents at increasing depths showing the variation trends of TOC/TOS ratio with depth, and (b) plot of H/C vs. O/C atomic ratios for thermal maturity assessment of the Liutitang Formation shales in Songtao, northern Guizhou

图3 黔北松桃地区ZK钻孔下寒武统牛蹄塘组页岩孔隙电镜照片 a—深度为1 322 m,有机质孔隙;b—深度为1 330 m,有机质孔隙;c—深度为1 331 m,晶间空隙;d—深度为1 333 m,粒间孔隙;e—深度为1 328 m,溶蚀孔隙;f—深度为1 323 m,有机质边缘微裂缝。

Fig.3 SEM images of shale samples from Well ZK in Songtao, northern Guizhou for pore structural characterization

表2 基于N2吸附数据的页岩孔隙结构参数与分形维数

Table 2 Pore structural parameters and pore fractal dimensions in shale samples based on N2 adsorption experiment

样品编号	比表面积/ (m²·g^-1)	总孔体积/ (cm³·g^-1)	平均孔径/ nm	孔径/ nm	p/p₀<0.45情况下			p/p₀>0.45情况下
样品编号	比表面积/ (m²·g^-1)	总孔体积/ (cm³·g^-1)	平均孔径/ nm	孔径/ nm	拟合系数 $R 2$	分形维数 $D 1$	分形维数D $' 1$	拟合系数 $R 2$	分形维数 $D 2$
ZK1	13.650	0.021 9	6.427	281.7	0.99	2.702 3	2.106 9	0.99	2.808 4
ZK2	14.765	0.019 0	5.148	284.8	0.99	2.703 7	2.111 1	0.99	2.834 2
ZK3	13.021	0.020 3	6.246	286.2	0.99	2.690 0	2.070 0	0.99	2.806 2
ZK4	14.715	0.019 5	5.292	289.6	0.99	2.678 1	2.034 3	0.99	2.822 7
ZK5	12.696	0.021 0	6.604	286.5	0.99	2.650 8	1.952 4	0.99	2.787 8
ZK6	12.139	0.021 3	7.025	294.4	0.99	2.677 6	2.032 8	0.99	2.799 5
ZK7	13.195	0.021 6	6.542	284.6	0.99	2.690 9	2.072 7	0.99	2.809 9
ZK8	11.954	0.019 8	6.631	279.4	0.99	2.691 6	2.074 8	0.99	2.814 1
ZK9	12.326	0.018 6	6.025	286.1	0.99	2.694 6	2.083 8	0.99	2.812 6
ZK10	13.041	0.020 7	6.360	283.1	0.99	2.687 4	2.062 2	0.99	2.804 9
ZK11	15.459	0.022 8	5.891	272.7	0.99	2.698 7	2.096 1	0.99	2.829 4
ZK12	14.491	0.021 8	6.020	279.8	0.99	2.688 3	2.064 9	0.99	2.814 1
ZK13	18.034	0.025 2	5.601	273.5	0.99	2.706 1	2.118 3	0.99	2.832 6
ZK14	17.348	0.021 4	4.923	352.1	0.99	2.700 7	2.102 1	0.99	2.842 7
ZK15	21.744	0.025 9	4.773	252.7	0.99	2.699 8	2.099 4	0.99	2.850 3

表2 基于N2吸附数据的页岩孔隙结构参数与分形维数

Table 2 Pore structural parameters and pore fractal dimensions in shale samples based on N2 adsorption experiment

样品编号	比表面积/ (m²·g^-1)	总孔体积/ (cm³·g^-1)	平均孔径/ nm	孔径/ nm	p/p₀<0.45情况下			p/p₀>0.45情况下
样品编号	比表面积/ (m²·g^-1)	总孔体积/ (cm³·g^-1)	平均孔径/ nm	孔径/ nm	拟合系数 $R 2$	分形维数 $D 1$	分形维数D $' 1$	拟合系数 $R 2$	分形维数 $D 2$
ZK1	13.650	0.021 9	6.427	281.7	0.99	2.702 3	2.106 9	0.99	2.808 4
ZK2	14.765	0.019 0	5.148	284.8	0.99	2.703 7	2.111 1	0.99	2.834 2
ZK3	13.021	0.020 3	6.246	286.2	0.99	2.690 0	2.070 0	0.99	2.806 2
ZK4	14.715	0.019 5	5.292	289.6	0.99	2.678 1	2.034 3	0.99	2.822 7
ZK5	12.696	0.021 0	6.604	286.5	0.99	2.650 8	1.952 4	0.99	2.787 8
ZK6	12.139	0.021 3	7.025	294.4	0.99	2.677 6	2.032 8	0.99	2.799 5
ZK7	13.195	0.021 6	6.542	284.6	0.99	2.690 9	2.072 7	0.99	2.809 9
ZK8	11.954	0.019 8	6.631	279.4	0.99	2.691 6	2.074 8	0.99	2.814 1
ZK9	12.326	0.018 6	6.025	286.1	0.99	2.694 6	2.083 8	0.99	2.812 6
ZK10	13.041	0.020 7	6.360	283.1	0.99	2.687 4	2.062 2	0.99	2.804 9
ZK11	15.459	0.022 8	5.891	272.7	0.99	2.698 7	2.096 1	0.99	2.829 4
ZK12	14.491	0.021 8	6.020	279.8	0.99	2.688 3	2.064 9	0.99	2.814 1
ZK13	18.034	0.025 2	5.601	273.5	0.99	2.706 1	2.118 3	0.99	2.832 6
ZK14	17.348	0.021 4	4.923	352.1	0.99	2.700 7	2.102 1	0.99	2.842 7
ZK15	21.744	0.025 9	4.773	252.7	0.99	2.699 8	2.099 4	0.99	2.850 3

图4 黔北松桃地区牛蹄塘组页岩N2吸脱附等温线 p0—饱和蒸气压,MPa;p—平衡压力,MPa。

Fig.4 Nitrogen adsorption-desorption isotherms for selected Liutitang Formation shale samples in Songtao, northern Guizhou

表3 基于压汞实验的黔北松桃地区牛蹄塘组页岩孔隙结构参数表

Table 3 Pore structural parameters for selected Liutitang Formation shale samples in Songtao, northern Guizhou based on mercury intrusion experiment

样品编号	深度/m	孔体积/(cm³·g^-1)			孔体积比例/%			孔隙度/ %		拟合系数 R²		分形维数 D_Hg
样品编号	深度/m	中孔 (50~200 nm)	大孔 (>200 nm)	总孔	中孔 (50~200 nm)	大孔 (>200 nm)		孔隙度/ %		拟合系数 R²		分形维数 D_Hg
ZK11	1 336.55	0.000 0	0.000 7	0.000 7	0	100	0.13		0.96		2.813 1
ZK12	1 337.35	0.000 0	0.000 5	0.000 5	0	100	0.12		0.95		2.474 7
ZK13	1 338.86	0.000 0	0.000 5	0.000 5	0	100	0.09		0.94		2.690 2
ZK14	1 339.03	0.000 4	0.000 4	0.000 8	50	50	0.16		0.87		2.216 1
ZK15	1 339.48	0.000 9	0.000 4	0.001 3	69	31	0.31		0.96		2.506 9

图5 黔北松桃地区牛蹄塘组页岩孔径分布图(以ZK11-ZK15为例) a—低温氮气吸附数据的孔隙分布;b—基于压汞数据的孔隙分布。

Fig.5 Pore size distribution plots for selected Liutitang Formation shale samples (ZK11-ZK15) in Songtao, northern Guizhou based on low-temperature nitrogen adsorption (a) and mercury injection data (b)

图6 基于氮气吸附的页岩样品孔隙结构的分形特征

Fig.6 FHH model fitting results for selected shale samples in nitrogen adsorption experiment, revealing the change of pore fractal dimensions in different pore-size ranges

图7 基于高压压汞数据的页岩孔隙分形特征蓝框区域前面部分代表相对压力较低时汞进入到样品裂隙中,蓝框后半部分为汞进入样品的表面孔隙,该阶段不反映样品内部孔隙结构;红框区域为汞开始进入页岩基质孔隙,对应孔径约3 000 nm,截止点为孔径200 nm;灰色区域表示汞进入孔径为50~200 nm孔隙中;绿色区域表示孔径<50 nm。考虑到高压压汞对小孔隙的测定精确度不高,研究仅针对200 nm以上孔隙的分形维数进行拟合。

Fig.7 Fractal analysis plots for selected shale samples in high-pressure mercury injection experiment, showing the multifractal characteristics

图8 黔北松桃地区牛蹄塘组页岩孔隙结构参数相关关系图 a—氮气吸附比表面积与孔隙体积;b—氮气吸附总孔隙体积与不同孔径孔隙体积;c—氮气吸附比表面积与平均孔径;d—压汞总孔体积与压汞孔隙度。

Fig.8 Correlation relationships between pore structural parameters of the Liutitang Formation shales in Songtao, northern Guizhou

图9 分形维数与孔隙结构参数之间的关系上面各小图分别显示分形维数D2与D1(a)、孔隙体积(b)和分形维数与平均孔径(c)、比表面积(d)的关系。

Fig.9 Relationship between fractal dimension and pore structural parameters

表4 黔北松桃地区牛蹄塘组页岩矿物含量、TOC含量、分形维数各参数间相关性分析

Table 4 Correlation matrix for mineral components and pore fractal dimensions of the Liutitang Formation shales in Songtao, northern Guizhou

参数	各参数间的相关系数
	矿物含量							TOC含量	D₁	D₂
	石英	钾长石	斜长石	方解石	白云石	黄铁矿	黏土矿物	TOC含量	D₁	D₂
矿物含量
石英	1
钾长石	-0.102	1
斜长石	-0.644	-0.128	1
方解石	0.423	0.085	-0.029	1
白云石	-0.639	-0.257	0.721	-0.202	1
黄铁矿	-0.609	0.106	0.296	-0.157	0.14	1
黏土矿物	-0.446	-0.418	0.079	-0.606	0.35	-0.179	1
TOC含量	-0.58	0.244	0.368	-0.555	0.156	0.573	0.076	1
D₁	-0.215	0.247	0.442	0.062	0.004	0.131	-0.162	0.317	1
D₂	-0.371	0.188	0.412	-0.247	0.05	0.521	-0.185	0.696	0.713	1

图10 黔北松桃地区牛蹄塘组页岩TOC含量与孔隙结构参数之间的关系上面各小图分别显示总有机碳(TOC)含量与孔隙比表面积(a)、平均孔径(b)、不同孔径孔隙体积(c)、分形维数(d)的关系。图a和b中焦石坝龙马溪组数据来自文献[21],四川牛蹄塘组数据来自文献[2],宜昌EYY1井数据来自文献[22]。

Fig.10 Relationship between TOC and pore structural parameters of the Liutitang Formation shales in Songtao, northern Guizhou

图11 不同类型页岩孔隙分形维数分布对比数据来源:(1)—文献[33];(2)—文献[21];(3)—文献[27];(4)—文献[29];(5)—文献[23];(6)—文献[11,28];(7)—文献[34];(8)—文献[35];(9)—文献[18];(10)—焦炭,文献[18];(11)—文献[32];(12)—文献[31];(13)—文献[30]。

Fig.11 Comparison of pore fractal dimensions between different shale formations

参考文献 38

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黔北寒武系牛蹄塘组页岩孔隙分形表征

Fractal characterization of pore structure in Cambrian Niutitang shale in northern Guizhou, southwestern China

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