Advances In Protein Chemistry And Structural Biology, Vol 121

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Advances In Protein Chemistry And Structural Biology, Vol 121

作者 Huang, Jingyao; Wang, Shuoyang; Jia, Yuxin; Zhang, Yujia; Dai, Xueyu; et al. 期刊 In the era of big data, the interplay of artificial and human intelligence is the demanding job to address the concerns involving exchange of decisions between both sides. Drug discovery is one of the key sources of the big data, which i... DOI 10.1016/s1876-1623(20)30012-2 类型 原创研究 (Original Research)

📄 英文摘要 English Abstract

EN

lTargeting FOXP3 complex ensemble in drug discovery

📄 中文摘要 Chinese Abstract

中文
中国陆相页岩具有优越的地质特征和巨大的资源潜力,但天然能量开采下的采收率仍然极低。研究陆相页岩中水力诱导层理裂缝形成复杂裂缝网络的机制,并建立有效渗流体系,具有极其重要的意义。松辽盆地古龙页岩油是陆相页岩油的典型代表,其特点是矿物组成复杂、物性差、层理裂缝发育。多段水平井压裂后,天然能量快速衰减,导致采收率仅约5%。在黏土含量高、层理裂缝发育的陆相页岩中,渗吸过程中会形成新的水力裂缝,注入流体通过水力诱导形成的页岩油渗流体系对高效开发起着关键作用。 前人研究表明,黏土矿物含量是影响页岩水化导致渗透率损害的主要因素,层理面会限制水力诱导裂缝的扩展高度。水化从根本上取决于黏土矿物含量和自由水侵入,而自由水侵入受毛细管效应、沿层理面和微裂缝侵入、孔隙压力传播以及化学反应的影响。中国陆相页岩油藏多为油湿或混合润湿,因此必须使用表面活性剂溶液或纳米流体来改变页岩表面的润湿性。因此,研究不同注入流体激活层理裂缝并建立有效渗流体系的机制,并明确其渗流能力和渗流行为,具有重要意义。

📋 英文结构化总结 English Structured Summary

全文整理

EN

Background:

China’s continental shale exhibits favorable geological characteristics and substantial resource potential, yet oil recovery for natural energy extraction remains critically low. Investigating the mechanisms of hydraulically induced bedding fracture to generate complex fracture networks in continental shale, and establishing effective flow systems, is of utmost importance. The Gulong shale oil in the Songliao Basin is a typical representative of continental shale oil, characterized by complex mineral composition, poor physical properties, and well-developed bedding fractures. After multi-stage horizontal well fracturing, natural energy rapidly declined, resulting in a low oil recovery of around 5%. In continental shales with high clay content and well-developed bedding fractures, new hydraulic fractures are formed during the imbibition process, and the shale oil flow system created by hydraulic induction through injected fluids plays a key role in efficient development.

Previous studies show that clay mineral content is a major factor influencing permeability damage due to hydration of shale, and that bedding planes restrict the height of hydraulically induced fracture propagation. Hydration fundamentally depends on the clay mineral content and free water invasion, which is influenced by capillary effects, intrusion along bedding planes and micro-fractures, pore pressure propagation, and chemical reactions. China’s continental shale oil reservoirs are oil-wet or mixed-wet, so surfactant solutions or nanofluids must be used to modify the wettability of shale surfaces. Therefore, it is crucial to investigate the mechanisms by which different injected fluids activate bedding fractures and establish effective flow systems, and to clarify the associated flow capacity and percolation behavior.

Methods:

Full-diameter shale cores from coring Well X of the Qingshankou Formation in the Songliao Basin were used. The cores were cut into cubic shale cores of 9 cm × 9 cm × 9 cm, placed in a 10 cm × 10 cm × 10 cm silicone mold, and encapsulated with epoxy resin adhesive. A 4.5 cm deep circular hole was drilled along the vertical bedding direction using an 8 mm drill bit, a 6 cm long steel pipe was inserted and fixed, and a 6 mm diameter drill bit was used to drill a 5.5 cm deep hole from the upper surface. The prepared fluids were a 0.75% KCl solution, a 0.1% CTAB solution, a 0.1% SiO2 solution, and a 0.1% mixed solution of CTAB and SiO2 (CTAB: SiO2 nanofluid = 1:1).

The prepared cores were placed in a true triaxial fracturing experimental apparatus, and a constant pressure of 8 MPa was applied in the x, y, and z directions. Fluid was injected at 10 mL/min until peak pressure was reached, then injected at flow rates of 0.5, 1, 2, 3, 4, 5, and 6 mL/min, with the flow rate adjusted every 2 min, and injection pressure was recorded. X-ray CT scanning was performed before and after fracture, and AVIZO software was used for fracture extraction. Numerical simulations used the Navier-Stokes equations for incompressible fluids, with inlet velocity 0.1 m/s, outlet pressure 0 Pa, no-slip shale surfaces, fluid viscosity 1 mPa·s, density 1000 kg/m3, and representative localized fractures of 5.3 mm length × 3.7 mm width.

Results:

When injecting KCl solution, the injection pressure reached 61.1 MPa and then dropped to 12.9 MPa; for CTAB solution, it reached 43.9 MPa and decreased to 4.5 MPa; for SiO2 solution, it reached 30.5 MPa and dropped to 3.3 MPa; for the CTAB and SiO2 mixed solution, it reached 57.3 MPa and decreased to 11.1 MPa. During subsequent rate tests, KCl solution showed significant pressure declines at 3 and 5 mL/min and a sharp drop at 6 mL/min, indicating detachment and migration of laminated shale fragments that supported preferential flow paths. CTAB solution and SiO2 solution maintained relatively stable flow capacity, while the mixed solution showed pressure drops at 2 and 4 mL/min and an initial decline followed by an increase at 6 mL/min, indicating particle migration, accumulation, and flushing. The final flow capacity order was SiO2 solution (S93) > CTAB solution (S148) > KCl solution (S156) > CTAB and SiO2 mixed solution (S132).

CT scanning showed that KCl solution formed a single distinct fracture, CTAB solution formed three clear fractures at different horizontal levels along the bedding planes, and no significant fractures were observed at the front position after SiO2 solution and mixed solution injection. Eroded and spalled shale fragments near the injection point were transported to farther locations, where they helped support localized fractures and increased fracture aperture. CTAB solution and SiO2 solution reduced shale surface hydration, preventing shale fragments from swelling and disintegrating, leading to more stable percolation behavior. The mixed solution produced relatively flat and smooth fracture surfaces that were prone to closure under confining pressure, reducing flow capacity.

Numerical simulations showed that velocity in the smaller flow paths near the closure was significantly higher than that in the main flow paths, leading to pronounced bypass flow behavior. The pressure difference increased progressively with increasing injection rate, and the rate of increase became more pronounced. At the same injection pressure, the fracture induced by the SiO2 solution exhibited the highest flow capacity. The flow capacities of the localized fractures induced by the KCl solution and the CTAB solution were relatively similar, with KCl solution showing higher flow capacity at low velocities (u < 0.3 m/s) and CTAB solution surpassing KCl solution when velocity exceeded 0.3 m/s. The lowest flow capacity was observed in the localized fractures induced by the CTAB and SiO2 mixed solution.

Data Summary:

The shale cores had porosity ranging from 3.7% to 4.2%, with an average of 4.0%, and horizontal permeability varying from 0.011 × 10−3 to 0.015 × 10−3 μm2, with an average of 0.013 × 10−3 μm2. The mineral composition was clay 54.2%, quartz 22.6%, and plagioclase 15.4%; the clay mineral composition was illite 59.7%, illite-montmorillonite mixed-layer 27.1%, and chlorite 9.7%. The fracture density was 500–1000 bedding fractures per meter.

The peak injection pressures were 61.1 MPa for KCl solution, 43.9 MPa for CTAB solution, 30.5 MPa for SiO2 solution, and 57.3 MPa for the CTAB and SiO2 mixed solution. The post-fracture pressure drops were to 12.9 MPa, 4.5 MPa, 3.3 MPa, and 11.1 MPa, respectively. The simulation grid numbers were 2,404,557 for S156, 3,625,455 for S148, 2,730,596 for S93, and 2,077,997 for S132. The flow capacity order from both experiments and simulations was SiO2 solution (S93) > CTAB solution (S148) and KCl solution (S156) > CTAB and SiO2 mixed solution (S132).

Conclusions:

The injection of different fluids hydraulically induced fracture opening along the shale bedding planes, forming an effective flow system. Shale fragments eroded and spalled near the injection end were transported to more distant locations and contributed to propping the fractures, increasing fracture openings and enhancing flow capacity. Both CTAB solution and SiO2 solution reduced shale surface hydration, stabilized the mechanical properties at the fracture interfaces, and made shale fragments less prone to swelling and disintegration, leading to more stable flow capacity.

The fracture flow capacities induced by CTAB solution and SiO2 solution were both higher than that induced by the CTAB and SiO2 mixed solution, because the coupling effect of the mixed solution severely inhibited shale hydration and prevented effective support of the fracture apertures. Hydraulic fractures induced by KCl solution, SiO2 solution, and the mixed solution each formed only a single fracture along the preferential shale bedding plane, while CTAB solution induced three distinct fractures at different horizontal levels. As the spatial distance from the shale fragments increases, the fractures gradually exhibit dispersed closure, and the velocity in the smaller flow paths near the closure is significantly higher than that in the main flow paths, resulting in a pronounced bypassing phenomenon that hinders effective fluid percolation through the shale core.

Practical Significance:

The results provide valuable insights into the mechanism of hydraulically induced bedding fracture in continental shale and offer guidance for the effective development of shale reservoirs. Using CTAB solution or SiO2 solution can reduce shale surface hydration, stabilize fracture contact surfaces, and maintain more stable flow capacity, which is important for improving production stability and maximizing recovery in continental shale oil reservoirs.

📋 中文结构化总结 Chinese Structured Summary

中文

背景:

中国陆相页岩具有优越的地质特征和巨大的资源潜力,但天然能量开采下的采收率仍然极低。研究陆相页岩中水力诱导层理裂缝形成复杂裂缝网络的机制,并建立有效渗流体系,具有极其重要的意义。松辽盆地古龙页岩油是陆相页岩油的典型代表,其特点是矿物组成复杂、物性差、层理裂缝发育。多段水平井压裂后,天然能量快速衰减,导致采收率仅约5%。在黏土含量高、层理裂缝发育的陆相页岩中,渗吸过程中会形成新的水力裂缝,注入流体通过水力诱导形成的页岩油渗流体系对高效开发起着关键作用。

前人研究表明,黏土矿物含量是影响页岩水化导致渗透率损害的主要因素,层理面会限制水力诱导裂缝的扩展高度。水化从根本上取决于黏土矿物含量和自由水侵入,而自由水侵入受毛细管效应、沿层理面和微裂缝侵入、孔隙压力传播以及化学反应的影响。中国陆相页岩油藏多为油湿或混合润湿,因此必须使用表面活性剂溶液或纳米流体来改变页岩表面的润湿性。因此,研究不同注入流体激活层理裂缝并建立有效渗流体系的机制,并明确其渗流能力和渗流行为,具有重要意义。

方法:

采用松辽盆地青山口组X取心井的全直径页岩岩心。将岩心切割成9 cm × 9 cm × 9 cm的立方体页岩岩心,放入10 cm × 10 cm × 10 cm的硅胶模具中,并用环氧树脂胶粘剂封装。沿垂直层理方向使用8 mm钻头钻一个深4.5 cm的圆孔,插入并固定一根长6 cm的钢管,再用直径6 mm的钻头从上表面钻一个深5.5 cm的孔。配制的流体包括0.75% KCl溶液、0.1% CTAB溶液、0.1% SiO2溶液以及0.1% CTAB和SiO2混合溶液(CTAB:SiO2纳米流体 = 1:1)。

将制备好的岩心放入真三轴压裂实验装置中,并在x、y、z方向施加8 MPa的恒定压力。以10 mL/min的流量注入流体,直至达到峰值压力,然后分别以0.5、1、2、3、4、5和6 mL/min的流量注入,每2 min调整一次流量,并记录注入压力。压裂前后进行X射线CT扫描,并使用AVIZO软件进行裂缝提取。数值模拟采用不可压缩流体的Navier-Stokes方程,入口速度为0.1 m/s,出口压力为0 Pa,页岩表面为无滑移边界,流体黏度为1 mPa·s,密度为1000 kg/m3,代表性局部裂缝尺寸为长5.3 mm × 宽3.7 mm。

结果:

注入KCl溶液时,注入压力达到61.1 MPa,随后降至12.9 MPa;注入CTAB溶液时,压力达到43.9 MPa,随后降至4.5 MPa;注入SiO2溶液时,压力达到30.5 MPa,随后降至3.3 MPa;注入CTAB和SiO2混合溶液时,压力达到57.3 MPa,随后降至11.1 MPa。在后续变流量测试中,KCl溶液在3 mL/min和5 mL/min时出现明显压力下降,在6 mL/min时出现急剧下降,表明支撑优势渗流通道的层状页岩碎片发生剥落和迁移。CTAB溶液和SiO2溶液保持了相对稳定的渗流能力,而混合溶液在2 mL/min和4 mL/min时出现压力下降,在6 mL/min时先下降后上升,表明颗粒发生迁移、聚集和冲刷。最终渗流能力排序为:SiO2溶液(S93)> CTAB溶液(S148)> KCl溶液(S156)> CTAB和SiO2混合溶液(S132)。

CT扫描显示,KCl溶液形成一条清晰的单一裂缝,CTAB溶液沿层理面在不同水平位置形成三条清晰裂缝,而SiO2溶液和混合溶液注入后在前端位置未观察到明显裂缝。注入点附近被侵蚀和剥落的页岩碎片被运移至更远处,有助于支撑局部裂缝并增大裂缝开度。CTAB溶液和SiO2溶液降低了页岩表面水化程度,防止页岩碎片膨胀和崩解,使渗流行为更加稳定。混合溶液形成的裂缝表面相对平整光滑,在围压作用下容易闭合,从而降低渗流能力。

数值模拟表明,闭合区附近较小渗流通道中的速度明显高于主渗流通道中的速度,导致明显的绕流现象。随着注入流量增加,压差逐渐增大,且增大速率更加明显。在相同注入压力下,SiO2溶液诱导形成的裂缝表现出最高的渗流能力。KCl溶液和CTAB溶液诱导形成的局部裂缝的渗流能力相对接近,其中KCl溶液在低流速(u < 0.3 m/s)下渗流能力较高,当流速超过0.3 m/s时,CTAB溶液的渗流能力超过KCl溶液。CTAB和SiO2混合溶液诱导形成的局部裂缝渗流能力最低。

数据汇总:

页岩岩心孔隙率为3.7%~4.2%,平均为4.0%;水平渗透率为0.011 × 10−3~0.015 × 10−3 μm2,平均为0.013 × 10−3 μm2。矿物组成为黏土54.2%、石英22.6%、斜长石15.4%;黏土矿物组成为伊利石59.7%、伊利石—蒙脱石混层27.1%、绿泥石9.7%。裂缝密度为每米500~1000条层理裂缝。

KCl溶液、CTAB溶液、SiO2溶液和CTAB与SiO2混合溶液的峰值注入压力分别为61.1 MPa、43.9 MPa、30.5 MPa和57.3 MPa。压裂后压力分别降至12.9 MPa、4.5 MPa、3.3 MPa和11.1 MPa。S156、S148、S93和S132的模拟网格数分别为2,404,557、3,625,455、2,730,596和2,077,997。实验和模拟得到的渗流能力排序均为:SiO2溶液(S93)> CTAB溶液(S148)和KCl溶液(S156)> CTAB和SiO2混合溶液(S132)。

结论:

不同流体的注入沿页岩层理面水力诱导裂缝开启,形成有效渗流体系。注入端附近被侵蚀和剥落的页岩碎片被运移至更远处,有助于支撑裂缝,增大裂缝开度并提高渗流能力。CTAB溶液和SiO2溶液均能降低页岩表面水化程度,稳定裂缝界面力学性质,使页岩碎片不易膨胀和崩解,从而保持更稳定的渗流能力。

CTAB溶液和SiO2溶液诱导形成的裂缝渗流能力均高于CTAB和SiO2混合溶液诱导形成的裂缝,因为混合溶液的耦合作用强烈抑制了页岩水化,并阻止裂缝开度得到有效支撑。KCl溶液、SiO2溶液和混合溶液诱导形成的水力裂缝均仅沿优势页岩层理面形成单一裂缝,而CTAB溶液在不同水平位置诱导形成三条明显裂缝。随着距页岩碎片空间距离的增加,裂缝逐渐呈现分散闭合特征,闭合区附近较小渗流通道中的速度明显高于主渗流通道中的速度,导致明显的绕流现象,阻碍流体在页岩岩心中有效渗流。

实际意义:

研究结果揭示了陆相页岩中水力诱导层理裂缝的机制,为页岩油藏的有效开发提供了指导。使用CTAB溶液或SiO2溶液可降低页岩表面水化程度,稳定裂缝接触面,并维持更稳定的渗流能力,这对提高陆相页岩油藏生产稳定性和最终采收率具有重要意义。

📖 英文全文 English Full Text

EN

Original Paper Study on flow capacity and percolation behavior of hydraulically induced bedding fracture by different fluids in full-diameter shale cores

Hong-Tao Fu a,b, Kao-Ping Song a, Er-Long Yang c, Yu Zhao d, Xi Xia e, Li-Hao Liang e,f,* a Unconventional Petroleum Research Institute, China University of Petroleum (Beijing), Beijing, 102249, China b School of Mechanics and Engineering Science, Peking University, Beijing, 100871, China c School of Petroleum Engineering, Northeast Petroleum University, Daqing, 163318, Heilongjiang, China d Research Institute of Exploration and Development of Daqing Oilfield Company Ltd., Daqing, 163712, Heilongjiang, China e School of Petroleum Engineering, China University of Petroleum (Beijing), Beijing, 102249, China f Research Institute of Petroleum Exploration & Development, Beijing, 100083, China a r t i c l e i n f o

Article history:

Received 18 January 2025 Received in revised form 22 September 2025

Accepted 22 September 2025 Available online 25 September 2025

Edited by Jia-Jia Fei Keywords:

Shale Fracture extension Bedding fracture Flow capacity

Fluid percolation a b s t r a c t Chinaʼs continental shale exhibits favorable geological characteristics and substantial resource potential, yet oil recovery for natural energy extraction remains critically low. Investigating the mechanisms of hydraulically induced bedding fracture to generate complex fracture networks in continental shale, and establishing effective flow systems, is of utmost importance. This study employs laboratory experiments and numerical simulations to investigate the flow capacity and percolation behavior of hydraulically induced bedding fractures by different fluids in full-diameter shale cores. Hydraulic stimulation using different fluids generates bedding plane fracture networks, establishing effective flow systems. Eroded and detached shale fragments support localized fractures, thereby increasing their opening and enhancing flow capacity. Cetyltrimethylammonium bromide (CTAB) solution and SiO2 solution reduce the hydration of the shale surface, preventing shale fragments from swelling and disintegrating, leading to more stable percolation behavior. Eroded and spalled shale fragments near the injection point are transported to farther locations, where they help support localized fractures. This process differs from conventional hydraulic fracturing. Under a constant injection rate, the velocity in the smaller flow paths near the closure is significa cantly higher than that in the main flow paths, leading to pronounced bypass flow behavior. This restricts the percolation of fluid during imbibition in shale cores. The results provide valuable insights into the mechanism of hydraulically induced bedding fracture in continental shale, offering guidance for the effective development of shale reservoirs.

© 2025 The Authors. Publishing services by Elsevier B.V. on behalf of KeAi Communications Co. Ltd. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc- nd/4.0/).

1. Introduction In recent years, shale oil has emerged as another hotspot in global unconventional oil and gas exploration and development, following tight oil (Hu et al., 2020; Dou et al., 2022; Gao et al.,

2024). Globally, shale oil production, primarily from marine de- posits, has been rapidly expanding. The development of shale oil in the United States has played a pioneering role, triggering the global ʻshale oil revolutionʼ (Shakya et al., 2022; Kim et al., 2023;

Mcmahon et al., 2024). Unlike the marine deposits in the United

States, Chinaʼs shale oil resources are primarily from continental deposits.

Preliminary estimates suggest that the geological resource of mature shale oil in continental deposits is approxi- mately 200 × 108 t, with technically recoverable reserves reaching

43.9 × 108 t, about 54.7% of the technically recoverable reserves of conventional oil and gas (Zhou et al., 2023; EIA, 2013). These re- sources are primarily distributed in basins such as Songliao, Ordos, and Junggar (Yang et al., 2021; Wang et al., 2022a, 2022b; Zhao et al., 2024). With Chinaʼs growing energy demand, effici cient development of shale oil reservoirs has become one of the

* Corresponding author.

E-mail address: Petrolihao@163.com (L.-H. Liang).

Peer review under the responsibility of China University of Petroleum (Beijing).

Contents lists available at ScienceDirect Petroleum Science journal homepage: www.keaipublishing.com/en/journals/petroleum-science https://doi.org/10.1016/j.petsci.2025.09.035

1995-8226/© 2025 The Authors. Publishing services by Elsevier B.V. on behalf of KeAi Communications Co. Ltd. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

Petroleum Science 22 (2025) 5084–5096 effective solutions to address its current energy shortage. The

Chinese government is accelerating the effici cient development of continental shale oil to ensure its energy security.

The Gulong shale oil, located in China’s Songliao Basin, a typical representative of continental shale oil, has an estimated geological reserve of 12.7 × 108 t (Sun et al., 2023; Wang et al., 2023a, 2023b).

It is characterized by a complex mineral composition, poor phys- ical properties, and well-developed bedding fractures (He et al.,

2023; Sun et al., 2023; Wang et al., 2023a, 2023b; Meng et al.,

2024). As it is a novel resource type, no geological theories or development technologies derived from global experience can be directly applied, making the development process particularly challenging (Sun et al., 2021, 2023; Song et al., 2024). After the implementation of multi-stage horizontal well fracturing tech- nology in the continental shale of Songliao Basin, natural energy rapidly declined, resulting in a low oil recovery of around 5%.

Previous studies have shown that the application of imbibition by injected fluids significa cantly improves the recovery of shale oil reservoirs (Zhang et al., 2023a, 2023b; Guo et al., 2024). However, in continental shales with high clay content and well-developed bedding fractures, new hydraulic fractures are formed during the imbibition process (Lv and Hou, 2024; Zhao et al., 2024; Fu et al.,

2024). The shale oil flow system created by hydraulic induction through injected fluids plays a key role in the effici cient develop- ment of continental shale oil.

In recent years, the mechanism of hydraulically induced frac- turing in continental shale by injected fluids has become a research hotspot. Studies have shown that the clay mineral con- tent is a major factor influe uencing permeability damage due to hydration of shale. Significa cant damage occurs when the clay mineral content in shale exceeds 15% (Zhang et al., 2017). In shale with bedding fractures, the bedding planes restrict the height of hydraulically induced fracture propagation, with the fracture tips remaining within the bedding planes (Zhang et al., 2024a). He et al. (2020) further proposed that hydraulically induced micro- fractures primarily propagate along the mineral-organic matter interfaces. Zhuang et al. (2014) found that significa cant dissolution occurred during the water-shale interaction, promoting the for- mation of new fractures. The dissolution of shale is primarily caused by carbonate minerals, such as calcite. Ma et al. (2016) suggested that shale hydration fundamentally depends on the clay mineral content and free water invasion. Water invasion is influ- u- enced by capillary effects, intrusion along bedding planes and micro-fractures, pore pressure propagation, chemical reactions, and other processes. In these studies, the injected fluids were either pure water or formation water. In contrast, Chinaʼs conti- nental shale oil reservoirs are oil-wet or mixed-wet (Wang et al.,

2022a, 2022b). To achieve spontaneous imbibition and enhance oil recovery, surfactant solutions or nanoflui uids must be used to modify the wettability of shale surfaces (Liu et al., 2019; Hou and

Sheng, 2022). Therefore, it is crucial to investigate the mechanisms by which different injected fluids activate bedding fractures and establish effective flow systems in continental shale. In addition, clarifying the associated flow capacity and percolation behavior is essential for improving production stability and maximizing re- covery in continental shale oil reservoirs.

In this study, full-diameter shale cores from the Songliao Basin were used to conduct experiments on hydraulic fracture propa- gation induced by different fluids, aiming to evaluate the flow capacity of the resulting fractures. Based on the experimental re- sults, numerical simulations were conducted to investigate the percolation behavior of different fluids within the hydraulically induced fractures.

2. Geological overview of coring well The Songliao Basin, located in northeastern China, trends northeast with a length of approximately 750 km and a width ranging from 330 to 370 km. It is a typical continental rift- depression lake basin and is considered one of the most resource-rich oil and gas basins in the world (Fig. 1(a)) (Li et al.,

2024; Yu et al., 2024; Xiao et al., 2024). The experimental cores were collected from the Qijia-Gulong Sag (Fig. 1(b)).

The Songliao Basin developed mainly during the Cretaceous, with large-scale lake transgressions occurring in the Late Creta- ceous, particularly during the deposition of the Qingshankou and

Nenjiang formations, leading to the widespread distribution of semi-deep to deep lacustrine deposits. In the Qingshankou For- mation, a major lake transgression formed a large and stable lake basin (Li et al., 2024; Yu et al., 2024; Xiao et al., 2024). Based on lithological and compositional characteristics, the main productive intervals of the shale formation (Q1 and lower Q2 members) are

Fig. 1. Location and lithology of coring Well X in the Songliao Basin: (a) Songliao Basin in northeastern China; (b) location of coring Well X in the Qijia-Gulong Sag; (c) lithology of the Qingshankou Formation in coring Well X (modified ed from Zhao et al., 2023).

H.-T. Fu, K.-P. Song, E.-L. Yang et al.

Petroleum Science 22 (2025) 5084–5096 5085 subdivided into nine oil layers, with a total thickness of 80–130 m (Fig. 1(c)) (Zhou et al., 2023). Full-diameter cores were obtained from the Q9 layer, which is classified ed as pure shale-type shale.

These cores exhibit well-developed bedding fractures, with rela- tively straight fracture surfaces and a fracture density of 500–1000 bedding fractures per meter.

3. Methodology 3.1. Experimental materials and methods

3.1.1. Materials The experimental materials included full-diameter shale cores from coring Well X of the Qingshankou Formation in the Songliao

Basin (diameter × length = 11 × 12 cm); silicone mold (length × width × height = 10 × 10 × 10 cm); deionized water; KCl (Shanghai Aladdin Biochemical Science and Technology Co., Ltd., purity≥99.98%); CTAB (Shanghai Aladdin Biochemical Science and

Technology Co., Ltd., purity≥99.0%); SiO2 nanoflui uid stock solution (prepared by the China University of Petroleum (East China), average particle size = 6 nm); epoxy resin adhesive (AB crystal adhesive, mixed at a 3:1 ratio); acrylic structural AB adhesive (Germany Kisling Company, mixed at a 1:1 ratio); steel pipe (outer diameter = 8 mm, inner diameter = 6 mm).

3.1.2. Methods (1) Core sample preparation ①The full-diameter cores (Fig. 2(d)) were cut into cubic shale cores with dimensions of 9 cm × 9 cm × 9 cm using a wire-cutting apparatus, and each was placed into a silicone mold.

Cylindrical shale cores (diameter × length = 2.5 × 4 cm) were machined from the remaining shale material, with horizontal air permeability and porosity subsequently measured through laboratory tests.

②The cubic shale core was placed at the center of a

10 cm × 10 cm × 10 cm silicone mold. Epoxy resin ad- hesive was then poured into the mold and cured for 24 h (Fig. 2(f)). To prevent deformation of the mold, acrylic plates were used to secure it. The encapsulated core was designed to fit into a 10 cm × 10 cm × 10 cm core holder.

Additionally, the epoxy resin layer prevented mechanical damage to the sample during subsequent drilling and pressure release.

③The encapsulated shale core was removed, and a 4.5 cm deep circular hole was drilled along the vertical bedding direction using an 8 mm drill bit.

④A 6 cm long steel pipe was inserted into the hole and fixed using acrylic structural AB resin, then cured for

24 h.

⑤A 6 mm diameter drill bit was used to drill a 5.5 cm deep hole, from the upper surface of the core, completing the core preparation after encapsulation and tube insertion (Fig. 2(e)). (2) Hydraulically induced fracture expansion experiment

①The cubic shale cores were scanned and reconstructed using an X-ray CT scanner before the steel pipe was fixed following drilling. The resolution of the CT scan was

53 μm.

②A 0.75% (mass fraction) KCl solution was prepared, using the KCl solution as the base fluid, a 0.1% CTAB solution, a

0.1% SiO2 solution, and a 0.1% mixed solution of CTAB and

SiO2 (CTAB: SiO2 nanoflui uid = 1:1) were prepared.

③The prepared fluid was introduced into the intermediate container, the outlet end was closed, and the device was checked for leakage.

④The core, after encapsulation and tube insertion, was placed in the core chamber of the true triaxial fracturing experimental apparatus, and a constant pressure of

8 MPa was applied in the x, y, and z directions.

⑤The fluid was injected into the shale core at a flow rate of

10 mL/min until the peak pressure was reached.

⑥The fluid was injected at flow rates of 0.5, 1, 2, 3, 4, 5, and

6 mL/min, with the flow rate adjusted every 2 min, and the injection pressure was recorded.

Fig. 2. Experimental equipment and prepared cores: (a) true triaxial hydraulic fracturing experimental system; (b) nanoVoxel 3000 X-ray CT scanner (resolution: 0.5 μm); (c)

D8AA25 high-resolution X-ray diffractometer (Bruker, Germany); (d) full-diameter cores from coring Well X; (e) core preparation process for hydraulic fracturing; (f) cubic shale cores coated with epoxy resin adhesive.

H.-T. Fu, K.-P. Song, E.-L. Yang et al.

Petroleum Science 22 (2025) 5084–5096 5086 ⑦The steel pipe inside the core was removed, and the core was scanned and reconstructed using an X-ray CT scan- ner again. AVIZO software was used for fracture extrac- tion (Avizo, 2019). CT scanning was performed in accordance with Microbeam Analysis—Computer Tomog- raphy (CT) Imaging Method for Micro-Nanopore Structure of Tight Rocks (GB/T 38531-2020).

3.2. Numerical simulation 3.2.1. Simulation method (1) Governing equations

For viscous fluids, the velocity (u), pressure (p), and density (ρ) at any point in space satisfy the continuity equation based on mass conservation:

∂ρ ∂t + ∇⋅(ρu) = 0 (1) where ∇⋅(ρu) = ∂ρux ∂x + ∂ρuy

∂y + ∂ρuz ∂z (2) For incompressible fluids, the density remains constant over time and space. Therefore, the continuity equation simplifies es to:

∇⋅u = 0 (3) Let the body force per unit volume be F and the surface stress per unit volume be ∇⋅σ. According to Newtonʼs second law: ρ Du

Dt = ρF + ∇⋅σ (4) where σ is the total stress. σ = −pI + τ (5)

Du Dt is the particle acceleration:

Du Dt = ∂ ∂t u + (u ⋅∇)u (6) For elastic solids, the relationship between deformation and stress follows Hookeʼs law, while for viscous fluids, it follows

Stokesʼ law. τ = μ ( ∇u + ∇uT) (7) Based on the derivation of the continuity equation and New- tonʼs second law, the Navier-Stokes equation for incompressible fluids can be obtained under the assumption of negligible gravity.

The steady-state flow within the fractures is solved by using the

Navier-Stokes equations (Panton, 2013).

⎧ ⎨ ⎩ ρ [∂u ∂t + (u⋅∇)u ] = ∇ ( −pI + μ[∇u + (∇u)T])

∇u = 0 (8) where ρ is fluid density, kg/m3; u is fluid velocity, m/s; t is time, s; p is fluid pressure, Pa; I is identity matrix; μ is fluid viscosity, Pa⋅s. (2) Boundary conditions

The boundary conditions for each model are as follows: the left side is the inlet and the right side is the outlet, with specified ed velocities at the inlet. The outlet pressure is set to 0, and the shale surface is treated as a no-slip boundary.

Inlet boundary condition: u = u0; n⋅μ ( ∇u + (∇u)T )

= 0 (9) Outlet boundary condition: p = p0; n⋅μ ( ∇u + (∇u)T )

= 0 (10) Solid wall boundary: u = 0 (11) where n is the unit normal vector.

3.2.2. Model design and assumption (1) Model design

In the simulation process, the viscosity of the injected fluid was

1 mPa⋅s, and its density was 1000 kg/m3. The injection velocity was 0.1 m/s, and the outlet pressure was 0 Pa The hydraulically induced fractures of different fluids in the experiment were extracted using Avizo software (Avizo, 2019). For the numerical simulations, representative localized fractures corresponding to each fluid were selected, with dimensions of

5.3 mm (length) × 3.7 mm (width). The boundary layer thickness and mesh size of the partial fractures in each core were set to 5 μm. The total number of grids for each simulation case is listed in Table 1. (2) Model assumptions

This study employs a laminar flow model (Stokes flow) to simulate the percolation behavior of different fluids in micro- fractures within porous media. To simplify the computations, the following assumptions are made:

①The injected fluid is considered incompressible.

②The fluid is assumed to remain isothermal throughout the percolation process.

③All fluids are assumed to have identical density and viscosity.

④Gravitational effects are neglected due to the small scale of the model.

4. Results and discussion 4.1. Mineral composition and physical characteristics of shale cores

The mineral composition of shale influe uences its mineralization reactions and mechanical properties (Zhao et al., 2023; Zhou et al.,

2023; Hong et al., 2024). To characterize the physicochemical properties of the full-diameter shale samples used in this study, X- ray diffraction was employed to analyze the mineral composition of the core samples. The results are presented in Fig. 3(a) for overall mineral composition and Fig. 3(b) for clay mineral

Table 1 Mesh division for partial fractures in different shale cores.

Core number S156 S148 S93 S132 Fluid types KCl solution

CTAB solution SiO2 solution CTAB and SiO2 mixed solution

Number of grids 2404557 3625455 2730596 2077997 H.-T. Fu, K.-P. Song, E.-L. Yang et al.

Petroleum Science 22 (2025) 5084–5096 5087 composition. The shale primarily consists of clay minerals, quartz, and plagioclase, with clay accounting for 54.2%, quartz 22.6%, and plagioclase 15.4%. Compared to shale oil reservoirs in other basins, the clay mineral and plagioclase contents are relatively higher (Zhou et al., 2023). The clay mineral composition is dominated by illite, illite-montmorillonite mixed-layer, and chlorite. The illite content is 59.7%, illite-montmorillonite mixed-layer content is

27.1%, and chlorite content is 9.7%. The shale in the Songliao Basin has undergone advanced diagenesis, resulting in the trans- formation of montmorillonite into illite and the concurrent pre- cipitation of silica, thereby enhancing the rigidity and brittleness of the shale (Sun et al., 2021).

The porosity of the full-diameter shale cores ranges from 3.7% to 4.2%, with an average of 4.0% (Fig. 3(c)). The horizontal permeability varies from 0.011 ×10−3 to 0.015 × 10−3 μm2, with an average of 0.013 × 10−3 μm2 (Fig. 3(d)). These porosity and permeability values indicate poor reservoir quality. Macroscopic observations reveal numerous bedding fractures on the shale surface, which may facilitate fluid invasion along these natural fractures (Sun et al., 2023; Shi et al., 2023).

4.2. Experiment on hydraulically induced fractures

The variation characteristics of injection pressure curves are essential for understanding hydraulic fracture propagation in shale (Yang et al., 2022, 2023; Li et al., 2023). The time-pressure curves of hydraulically induced fractures in full-diameter shale cores with different fluids are shown in Fig. 4. When injecting KCl solution, the injection pressure reached 61.1 MPa, inducing hydraulic fracturing along the bedding planes, followed by a sharp drop to 12.9 MPa (Fig. 4(a)). For the CTAB solution, the injection pressure reached

43.9 MPa, inducing hydraulic fracturing along the bedding planes, and then the injection pressure rapidly decreased to 4.5 MPa (Fig. 4 (b)). When injecting the SiO2 solution, the injection pressure reached 30.5 MPa, inducing hydraulic fracturing along the bedding planes, followed by a rapid drop to 3.3 MPa (Fig. 4(c)). When injecting the CTAB and SiO2 mixed solution, the injection pressure reached 57.3 MPa, inducing hydraulic fracturing along the bedding planes, and subsequently decreased sharply to 11.1 MPa (Fig. 4(d)).

Generally, when the injection pressure is below the breakdown pressure, the fluid fills the wellbore and undergoes wellbore stor- age and compression, leading to a gradual pressure increase. Once the fracture initiation pressure of the bedding is reached, the weakly cemented shale bedding planes are activated. The fluids then rapidly break through from the wellbore along the induced fractures toward the core edges and flow out, resulting in a sharp drop in injection pressure. It is noteworthy that significa cant differ- ences exist in the peak pressures required to initiate fractures in full-diameter shale cores through hydration induced by different fluids. These differences can be attributed to variations in the

Fig. 3. Mineral composition and porosity-permeability characteristics: (a) mineral content of core S148; (b) clay mineral content of S148; (c) permeability of different full- diameter cores; (d) porosity of different full-diameter cores.

H.-T. Fu, K.-P. Song, E.-L. Yang et al.

Petroleum Science 22 (2025) 5084–5096 5088 degree of hydration caused by the different fluids, and pre-existing damage of the internal bedding fractures. Additionally, after hy- draulic fracture propagation in full-diameter shale cores with CTAB solution and SiO2 solution, the injection pressure was influe uenced by the applied triaxial compressive stress and was lower than the triaxial stress. This suggests that internal fragmentation occurred within the core, with shale fragments supporting the fracture walls and preventing the closure of new induced fractures, thereby enhancing the coreʼs flow capacity.

After hydraulic fractures were induced in full-diameter shale cores by injecting different fluids, each fluid was subsequently injected at increasing rates. The injection rate was incremented every 2 min, and the pressure-time relationship for each fluid was recorded at 1 s intervals (Fig. 5). The hydraulic fractures induced during the experiment propagated through the full-diameter cores and extended to the core surfaces, where the fluid pressure at the fracture tips was atmospheric. A constant triaxial stress of 8 MPa was applied to the full-diameter core. The injection pressure re- flects the flow capacity of the induced fractures within the shale core. During the KCl solution injection, when the injection rate was increased to 5 mL/min, the injection pressure initially rose. How- ever, significa cant pressure declines were observed at both 3 and

5 mL/min injection rates (Fig. 5(a)). When the injection rate reached 6 mL/min, a sharp drop in injection pressure occurred.

This indicates that during KCl solution injection, the hydration and erosion effects caused the detachment and migration of larger laminated shale fragments within the preferential flow paths of the core fractures. These shale fragments supported the prefer- ential flow paths within the opened fractures and enhanced their flow capacity. When injecting CTAB solution, increasing the in- jection rate to 6 mL/min, resulted in a rise in injection pressure across all tested rates, while maintaining relatively stable flow capacity (Fig. 5(b)). This indicates that the hydraulically induced fractures created by CTAB solution injection possess stable internal structures, where eroded, spalled, and transported shale frag- ments support the localized open fractures, leading to more stable flow capacity. When injecting the SiO2 solution, increasing the injection rate to 6 mL/min resulted in fracture flow capacity that was relatively stable and similar to that observed with CTAB so- lution injection (Fig. 5(c)). This suggests that both the CTAB solu- tion and SiO2 solution further suppressed shale surface hydration compared to the KCl solution, leading to more stable mechanical properties at the fracture contact surfaces. Some studies have shown that hydration can significa cantly destabilize the surface stability and mechanical properties of shale (Cui et al., 2023; Hong et al., 2024). However, both CTAB and SiO2 can promote the contraction of clay interlayer spacing, enhance the stability of clay mineral crystals, and maintain their mechanical performance,

Fig. 4. Injection pressure-time relationships with different fluids: (a) core S156 injected with KCl solution; (b) core S148 injected with CTAB solution; (c) core S93 injected with

SiO2 solution; (d) core S132 injected with CTAB and SiO2 mixed solution.

H.-T. Fu, K.-P. Song, E.-L. Yang et al.

Petroleum Science 22 (2025) 5084–5096 5089 thereby inhibiting the transport of water molecules within the clay minerals (Shi et al., 2023; Karimi et al., 2023). When injecting the

CTAB and SiO2 mixed solution, increasing the injection rate to 2 and 4 mL/min resulted in a significa cant pressure drop in the later stages (Fig. 5(d)). However, at injection rates of 3 and 5 mL/min, the injection pressure continued to rise. When the injection rate reached 6 mL/min, the pressure exhibited an initial decline fol- lowed by an increase as the injection volume increased. This in- dicates that during the injection of CTAB and SiO2 mixed solution, the fluid continuously eroded and transported small detached particles of clay or quartz within the shale core. These mobilized particles subsequently migrated into the flow paths, where they accumulated and eventually blocked the paths.

When the injection pressure within the flow path gradually increases to a certain threshold, the blocked path is flushed open.

This results in a process of increasing and then decreasing flow capacity within the core. Therefore, the strong coupling effect between CTAB and SiO2 in the solution overly suppresses the hy- dration of shale, which affects the detachment of shale fragments.

As a result, the opened fractures are difficu cult to support effectively and are more prone to closure. A comprehensive comparison of the final flow capacities within hydraulically induced fractures for different fluids reveals the following order:

SiO2 solution (S93) > CTAB solution (S148) > KCl solution (S156) > CTAB and SiO2 mixed solution (S132).

To investigate the actual fracture propagation induced by different fluids, CT scanning was performed to compare the pre- and post-fracture states of full-diameter shale cores subjected to hydraulic fracture propagation. The reconstructed surface states of the shale cores are shown in Fig. 6. From the reconstructed images of the cores, it was observed that after the KCl solution was injec- ted, a single distinct fracture was formed at the front position of the core. This phenomenon was observed by comparing region I (Fig. 6 (a)) to region II (Fig. 6(b)). In contrast, after the CTAB solution was injected, three clear fractures were formed at the front position of the core. This was observed by comparing region III (Fig. 6(c)) to region V (Fig. 6(d)) and region IV (Fig. 6(c)) to region VI (Fig. 6(d)).

No significa cant fractures were observed at the front position of the core after the SiO2 solution and the CTAB and SiO2 mixed solution were injected. This indicates that the full-diameter shale cores exhibit significa cant heterogeneity in the bedding direction, with no obvious pattern in the position of fluid penetration across the core.

However, it is notable that the fractures induced by KCl solution and CTAB solution are parallel to the bedding planes.

To further investigate the morphology of hydraulic fractures induced by different fluids, a brightness segmentation method was employed to extract the fracture networks (Zhang et al., 2024b).

The resulting fracture distributions in shale cores induced by various fluids are presented in Fig. 7. It was found that hydraulic fractures induced by KCl solution, SiO2 solution, and CTAB and SiO2

Fig. 5. Injection pressure-time relationships for different fluids after fracture initiation in full-diameter cores: (a) core S156 with KCl solution; (b) core S148 with CTAB solution; (c) core S93 with SiO2 solution; (d) core S132 with CTAB and SiO2 mixed solution.

H.-T. Fu, K.-P. Song, E.-L. Yang et al.

Petroleum Science 22 (2025) 5084–5096 5090 mixed solution propagated only along a single bedding direction (Fig. 7(a–e), and (g)). The resulting fractures were relatively smooth with no significa cant change in fracture trajectory. In contrast, hydraulic fractures induced by CTAB solution formed three distinct fractures at different horizontal levels along the bedding planes (Fig. 7(c)). The induced fractures extended only in one direction, with no observed activation on the opposite side. As the distance from the injection point increased, the fracture aperture grew. This further suggests that eroded shale fragments or small particles near the injection point were transported to greater distances, supporting the localized fractures. The aperture of these fractures increased, thereby enhancing their flow capacity.

This phenomenon was clearly visible in the magnified ed images of localized fractures induced by each fluid. These fractures represent localized connectivity, forming complex flow regions. However, the flow patterns within these regions are irregular, and the flow behavior at different locations along the fractures remains difficu cult to predict.

After hydraulic fracturing of full-diameter cores with different fluids, observations of the upper and lower fracture surfaces revealed the presence of laminated shale fragments at localized positions.

These shale fragments were observed at regions I–V (Fig. 8(a–e)).

These shale fragments constitute a self-supporting flow system within the shale cores. It was found that fractures induced by the hydraulic effect of the CTAB solution not only propagated along the horizontal bedding planes but also exhibited localized book-like fractures in the vertical direction. The phenomenon was observed at region VI in Fig. 8(g). This complex fracture pattern resulted in not only shale fragment-supported fractures (Fig. 8(k)) but also slip- supported fractures (Fig.

8(i)) within the core, significa cantly Fig. 6. 3D reconstructed images of hydraulically induced fractures by different fluids in full-diameter cores: (a) core S156 before KCl solution injection; (b) core S156 after KCl solution injection; (c) core S148 before CTAB solution injection; (d) core S148 after CTAB solution injection; (e) core S93 before SiO2 solution injection; (f) core S93 after SiO2 solution injection; (g) core S132 before CTAB and SiO2 mixed solution injection; (h) core S132 after CTAB and SiO2 mixed solution injection.

Fig. 7. Hydraulically induced fractures after injection of different fluids: (a) core S156 after KCl solution injection; (b) partial enlargement of (a); (c) core S148 after CTAB solution injection; (d) partial enlargement of (c); (e) core S93 after SiO2 solution injection; (f) partial enlargement of (e); (g) core S132 after CTAB and SiO2 mixed solution injection; (h) partial enlargement of (g).

H.-T. Fu, K.-P. Song, E.-L. Yang et al.

Petroleum Science 22 (2025) 5084–5096 5091 enhancing the anisotropic flow capacity of the fractures. Addition- ally, the areas of fragment detachment on the fracture surfaces formed potential preferential flow paths, thereby further enhancing the flow capacity. In contrast, the fracture surfaces induced by the

CTAB and SiO2 mixed solution appeared relatively flat and smooth, which resulted in better matching between the upper and lower fracture surfaces of the small particle-supported fracture. These flat and smooth fracture surfaces were prone to closure under confini ning pressure (Fig. 8(e)), significa cantly reducing the flow capacity. It is noteworthy that numerous small particles were observed on the fracture surfaces, further confirm rming that particle migration and accumulation cycles led to significa cant fluctuations in flow capacity during injections at different rates (Fig. 8(l)).

4.3. Simulation of percolation in hydraulically induced fractures

The velocity fields of localized fractures induced by different fluids in full-diameter shale cores are shown in Fig. 9. These frac- tures correspond to the localized hydraulically induced fractures shown in Fig. 7. It was found that the flow paths of localized frac- tures induced by KCl solution and CTAB solution gradually converged from a dendritic structure into a unified ed flow region, and their flow capacity increased progressively (Fig. 9(a–d)). This is due to the supporting effect of shale fragments around the unified ed flow region, while fractures at more distant locations tend to close in a scattered manner. The flow paths of localized fractures induced by the SiO2 solution evolve from one dispersed dendritic structure to another. This behavior occurs because shale fragments provide structural support in the middle section of the fracture, while the fracture gradually closes in a scattered manner as the distance from these fragments increases. In localized fractures induced by the

CTAB and SiO2 mixed solution, only a narrow flow path was present in the middle and at the edge, severely restricting fluid flow in these fractures. It is observed at region VII in Fig. 9(d). The velocity in the narrower flow paths near the localized contact surface was signif- icantly higher compared to that in the main flow paths. This phe- nomenon was observed at regions I (Fig. 9(a)), III (Fig. 9(b)), V and VI (Fig. 9(c)). As the flow path widens, the velocity decreases radially in localized areas, and the fluid gradually converges into the larger flow path (Fig. 9(f)). This phenomenon is mainly attributed to the lack of shale fragment support within these localized fracture zones. Notably, at the blind ends of the local fractures induced by the KCl solution, the SiO2 solution, and the CTAB and SiO2 mixed solution, there is virtually no fluid movement, and the fluid shows a stagnant state within these regions. This was observed at regions II (Fig. 9(a)) and VIII (Fig. 9(d)).

The pressure fields and flow streamline fields of localized fractures in full-diameter shale cores induced by different fluids

Fig. 8. Fracture surfaces and supporting patterns in full-diameter cores after injection of different fluids: (a) upper surface after KCl solution injection; (b) lower surface after KCl solution injection; (c) upper surface after CTAB solution injection; (d) lower surface after CTAB solution injection; (e) upper surface after SiO2 solution injection; (f) lower surface after SiO2 solution injection; (g) upper surface after CTAB and SiO2 mixed solution injection; (h) lower surface after CTAB and SiO2 mixed solution injection; (i) closed fracture; (j) sliding fracture; (k) fragment-supported fracture; (l) particle-supported fracture.

H.-T. Fu, K.-P. Song, E.-L. Yang et al.

Petroleum Science 22 (2025) 5084–5096 5092 were obtained through numerical simulations (Fig. 10). The results demonstrate significa cant differences in pressure distribution and flow behavior among the different fluids within shale fractures. It was found that the localized fractures induced by the KCl solution exhibited higher injection pressure in the narrower flow paths in the upper-left region. The injected fluid converged toward the central area in a dendritic pattern and then dispersed again in branching flows, with a relatively gentle pressure gradient observed within the fracture network (Fig.10(a)). This is attributed to the relatively uniform aperture of localized fractures supported by shale fragments, which facilitates smooth fluid flow. In contrast, the CTAB solution formed localized dendritic flow paths in the lower-right region of the fractures (Fig. 10(b)). Under identical injection rate conditions, the pressure gradient exhibited signifi- - cant variations when the flow paths narrowed (Fig. 10(e)). This phenomenon results from strong fracture closure at this location, which constricted the flow pathways and consequently induced drastic changes in the pressure gradient. The SiO2 solution exhibited the most gradual pressure gradient within localized fractures (Fig. 10(c)), indicating that shale fragments uniformly supported the fractures at this location, enabling fluid flow with a stable pressure gradient. This uniform self-supporting effect effectively prevents fracture closure, thereby maintaining high flow capacity. The CTAB and SiO2 mixed solution form only a minor flow path at the edge of the central fracture zone (Fig. 10(f)), resulting in concentrated injection pressure at this location. It is observed at region II in Fig. 10(d). The injection pressure decreases rapidly after passing through this constriction, exhibiting a radial diffusion pattern. This phenomenon was observed at region II in

Fig. 10(d). This indicates that the localized fractures at this loca- tion lack internal support from shale fragments, while the accu- mulation of fine particles within the preferential flow paths severely impedes fluid movement.

To quantitatively investigate the relationship between injection rate and pressure difference in fractures hydraulically induced by different fluids, the variation in pressure difference between the injection and outlet ends of localized fractures was analyzed under varying injection rates. It was found that within the localized fractures of each core, the pressure difference increased progres- sively with increasing injection rate, and the rate of increase also became more pronounced. At the same injection pressure, the fracture induced by the SiO2 solution exhibited the highest flow capacity. The flow capacities of the localized fractures induced by the KCl solution and the CTAB solution were relatively similar.

Notably, at low velocities (u < 0.3 m/s), the fracture induced by the

KCl solution exhibited higher flow capacity. However, when the velocity exceeded 0.3 m/s, the flow capacity of the fractures induced by the CTAB solution gradually surpassed that of the fracture induced by the KCl solution.

The lowest flow capacity was observed in the localized frac- tures induced by the CTAB and SiO2 mixed solution (Fig. 11(a)).

Simulation results show that the flow capacity of localized frac- tures by each fluid follows the order: SiO2 solution (S93) > CTAB solution (S148) and KCl solution (S156) > CTAB and SiO2 mixed

Fig. 9. Velocity fields in localized 3D fractures hydraulically induced by different fluids: (a) KCl solution; (b) CTAB solution; (c) SiO2 solution; (d) CTAB and SiO2 mixed solution; (e) enlarged view of V in (c); (f) enlarged view of VI in (b).

H.-T. Fu, K.-P. Song, E.-L. Yang et al.

Petroleum Science 22 (2025) 5084–5096 5093 solution (S132), which is consistent with the experimental results (Fig. 11(b)).

4.4. Discussion The continental shale in the Songliao Basin is characterized by abundant layering (also known as bedding fracture), which rep- resents the inherent micro-damage prior to shale hydration. For geotechnical structures with initial damage, the injection of fluids can induce new micro-damage at these pre-existing damaged sites. As micro-damage accumulates, it gradually evolves into macro-fractures, ultimately forming an effective fracture flow system. Additionally, the micro-structure of the shale bedding surfaces and sections also has a significa cant effect on the flow ca- pacity of shale.

In continental shale reservoirs with extremely low perme- ability, pore sizes are typically at the nanoscale. Additionally, the shale of the Songliao Basin is typically an oil-wet reservoir (Sun

Fig. 10. Pressure and flow streamline fields in localized 3D fractures hydraulically induced by different fluids: (a) KCl solution; (b) CTAB solution; (c) SiO2 solution; (d) CTAB and

SiO2 mixed solution; (e) enlarged of I in (b); (f) enlarged view of II in (d).

Fig. 11. (a) Injection pressure-velocity relationships for different fluids; (b) Injection pressure at 0.4 m/s.

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Petroleum Science 22 (2025) 5084–5096 5094 et al., 2021; Zhang et al., 2023a, 2023b), resulting in poor water imbibition capability of the shale matrix, which in turn inhibits the flow of the injected fluids within the shale matrix. Clay minerals are protected by CTAB and SiO2 nanoparticles, reducing hydration effects and making fractured shale debris less prone to swelling and disintegration. This stabilization helps maintain a more consistent flow capacity.

Moreover, fractures hydraulically induced by fluids gradually become essential paths for shale oil to flow from matrix pores to the wellbore.

5. Conclusions In this study, the flow capacity of fractures hydraulically induced by different fluids in full-diameter shale cores from the

Songliao Basin, China. The percolation behavior of the injected fluids in the hydraulically induced fractures was clarified ed. The main conclusions are summarized as follows: (1) The injection of different fluids hydraulically induced frac- ture opening along the shale bedding planes, forming an effective flow system. The fracture surfaces were relatively flat and smooth, and no obvious fracture turning was observed. (2) Shale fragments eroded and spalled near the injection end were transported to more distant locations and contributed to propping the fractures. The fracture openings at these locations increased, and the flow capacity was enhanced.

This behavior differs from that observed in conventional hydraulic fracturing. (3) Both the CTAB solution and the SiO2 solution reduced shale surface hydration, which stabilized the mechanical proper- ties at the fracture interfaces. As a result, shale fragments were less prone to swelling and disintegration, leading to a more stable flow capacity. (4) The fracture flow capacities induced by the CTAB solution and the SiO2 solution were both higher than that induced by the CTAB and SiO2 mixed solution. The coupling effect of mixed solution severely inhibited shale hydration, making shale fragments less likely to detach, thereby preventing effective support of the fracture apertures. (5) Hydraulic fractures induced by injection of the KCl solution, the SiO2 solution, and the CTAB and SiO2 mixed solution each formed only a single fracture along the preferential shale bedding plane. In contrast, the CTAB solution induced the formation of three distinct fractures at different hori- zontal levels along the shale bedding plane. (6) As the spatial distance from the shale fragments increases, the fractures gradually exhibit dispersed closure. The ve- locity in the smaller flow paths near the closure is signifi- - cantly higher than that in the main flow paths, resulting in a pronounced bypassing phenomenon. This hinders effective fluid percolation through the shale core.

CRediT authorship contribution statement Hong-Tao Fu: Writing – original draft, Methodology, Investi- gation, Conceptualization. Kao-Ping Song: Writing – review & editing, Supervision, Resources, Funding acquisition. Er-Long

Yang: Software, Resources, Investigation. Yu Zhao: Resources,

Funding acquisition, Formal analysis. Xi Xia: Visualization, Su- pervision, Software, Conceptualization. Li-Hao Liang: Writing – review & editing, Methodology, Formal analysis.

Data availability statement The data that support the findings of this study are available from the corresponding author upon reasonable request.

Declaration of competing interest The authors declare no conflic ict of interest.

Acknowledgments This work is supported by the Frontier and Fundamental

Research of Active Nanoflui uids Flooding for Enhanced Oil Recovery through Discontinuous and Variable-circle Modes in High Tem- perature and High Salinity Offshore Oilfiel elds (U22B6005); National

Natural Science Foundation of China (No. 52274037); Study on Key

Issues of Enhanced Oil Recovery of Gulong Shale Oil (DQYT-2022- JS-761).

Appendix A. Supplementary data Supplementary data to this article can be found online at https://doi.org/10.1016/j.petsci.2025.09.035.

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Petroleum Science 22 (2025) 5084–5096 5096

📖 中文全文 Chinese Full Text

中文

以下是该论文的中文译文(保留关键技术术语,尽量符合石油工程/页岩油领域中文表达习惯):

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## 不同流体在全直径页岩岩心中水力诱导层理裂缝的导流能力与渗流行为研究

**Hong-Tao Fu** a,b,**Kao-Ping Song** a,**Er-Long Yang** c,**Yu Zhao** d,**Xi Xia** e,**Li-Hao Liang** e,f,*

a 中国石油大学(北京)非常规油气研究院,中国 北京 102249 b 北京大学力学与工程科学学院,中国 北京 100871 c 东北石油大学石油工程学院,中国 黑龙江 大庆 163318 d 大庆油田有限责任公司勘探开发研究院,中国 黑龙江 大庆 163712 e 中国石油大学(北京)石油工程学院,中国 北京 102249 f 中国石油勘探开发研究院,中国 北京 100083

### 文章信息

**文章历史:** 收稿日期:2025年1月18日 修改稿收稿日期:2025年9月22日 接受日期:2025年9月22日 在线发表日期:2025年9月25日 编辑:Jia-Jia Fei

**关键词:** 页岩;裂缝延伸;层理裂缝;导流能力;流体渗流

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### 摘要

中国陆相页岩具有优越的地质特征和巨大的资源潜力,但依靠天然能量开采的采收率仍然极低。研究水力诱导层理裂缝在陆相页岩中形成复杂裂缝网络并建立有效渗流系统的机制,具有极其重要的意义。本研究采用实验室实验和数值模拟方法,研究不同流体在全直径页岩岩心中水力诱导层理裂缝的导流能力与渗流行为。采用不同流体进行水力压裂可形成层理面裂缝网络,建立有效渗流系统。被侵蚀和剥落的页岩碎屑对局部裂缝起支撑作用,从而增大裂缝开度并提高导流能力。十六烷基三甲基溴化铵(CTAB)溶液和SiO₂溶液可降低页岩表面水化程度,防止页岩碎屑膨胀和崩解,使渗流行为更加稳定。注入点附近被侵蚀和剥落的页岩碎屑被运移至更远处,有助于支撑局部裂缝。该过程不同于常规水力压裂。在恒定注入速率下,闭合区附近较小流道中的流速明显高于主流道中的流速,导致显著的绕流现象。这限制了页岩岩心中渗吸过程中流体的渗流。研究结果对认识陆相页岩中水力诱导层理裂缝的机制具有重要价值,可为页岩油藏的有效开发提供指导。

© 2025 作者。Elsevier B.V. 代表 KeAi Communications Co. Ltd. 提供出版服务。本文为开放获取文章,采用 CC BY-NC-ND 许可协议(http://creativecommons.org/licenses/by-nc-nd/4.0/)。

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## 1. 引言

近年来,页岩油继致密油之后成为全球非常规油气勘探开发的又一热点(Hu et al., 2020; Dou et al., 2022; Gao et al., 2024)。全球页岩油产量主要来自海相沉积,且正在快速扩张。美国页岩油开发发挥了先行作用,引发了全球“页岩油革命”(Shakya et al., 2022; Kim et al., 2023; Mcmahon et al., 2024)。与美国海相沉积不同,中国页岩油资源主要来自陆相沉积。

初步估算表明,陆相沉积成熟页岩油的地质资源量约为 200 × 10⁸ t,技术可采储量达 43.9 × 10⁸ t,约为常规油气技术可采储量的 54.7%(Zhou et al., 2023; EIA, 2013)。这些资源主要分布在松辽、鄂尔多斯和准噶尔等盆地(Yang et al., 2021; Wang et al., 2022a, 2022b; Zhao et al., 2024)。随着中国能源需求不断增长,页岩油藏的高效开发已成为解决当前能源短缺问题的有效途径之一。中国政府正在加快陆相页岩油的高效开发,以保障能源安全。

位于中国松辽盆地的古龙页岩油是陆相页岩油的典型代表,其估算地质储量为 12.7 × 10⁸ t(Sun et al., 2023; Wang et al., 2023a, 2023b)。其特点是矿物组成复杂、物性差、层理裂缝发育(He et al., 2023; Sun et al., 2023; Wang et al., 2023a, 2023b; Meng et al., 2024)。作为一种新型资源类型,全球经验形成的地质理论或开发技术均无法直接套用,使其开发过程极具挑战性(Sun et al., 2021, 2023; Song et al., 2024)。在松辽盆地陆相页岩实施多级水平井压裂技术后,天然能量迅速衰减,导致采收率较低,约为 5%。

已有研究表明,注入流体的渗吸作用可显著提高页岩油藏采收率(Zhang et al., 2023a, 2023b; Guo et al., 2024)。然而,在高黏土含量、层理裂缝发育的陆相页岩中,渗吸过程中会形成新的水力裂缝(Lv and Hou, 2024; Zhao et al., 2024; Fu et al., 2024)。通过注入流体水力诱导形成的页岩油渗流系统在陆相页岩油高效开发中起着关键作用。

近年来,注入流体在陆相页岩中诱导水力裂缝的机制已成为研究热点。研究表明,黏土矿物含量是影响页岩水化导致渗透率损伤的主要因素。当页岩中黏土矿物含量超过 15% 时,会发生显著损伤(Zhang et al., 2017)。在具有层理裂缝的页岩中,层理面会限制水力诱导裂缝的垂向延伸,裂缝尖端保持在层理面内(Zhang et al., 2024a)。He et al.(2020)进一步提出,水力诱导微裂缝主要沿矿物—有机质界面扩展。Zhuang et al.(2014)发现,水—页岩相互作用过程中会发生显著溶解,促进新裂缝形成。页岩的溶解主要由方解石等碳酸盐矿物引起。Ma et al.(2016)认为,页岩水化从根本上取决于黏土矿物含量和自由水侵入。水侵入受毛细管效应、沿层理面和微裂缝侵入、孔隙压力传播、化学反应等过程影响。在上述研究中,注入流体为纯水或地层水。相比之下,中国陆相页岩油藏多为油湿或混合湿(Wang et al., 2022a, 2022b)。为实现自发渗吸并提高采收率,必须使用表面活性剂溶液或纳米流体来改变页岩表面润湿性(Liu et al., 2019; Hou and Sheng, 2022)。因此,研究不同注入流体激活层理裂缝并在陆相页岩中建立有效渗流系统的机制至关重要。此外,明确相关导流能力和渗流行为,对于提高陆相页岩油藏生产稳定性、实现最大采收率也必不可少。

本研究采用松辽盆地全直径页岩岩心,开展不同流体诱导水力裂缝扩展实验,旨在评价所形成裂缝的导流能力。基于实验结果,开展数值模拟,研究不同流体在水力诱导裂缝中的渗流行为。

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## 2. 取心井地质概况

松辽盆地位于中国东北部,呈东北向展布,长约 750 km,宽 330–370 km。它是一个典型的陆相断陷湖盆,被认为是世界上油气资源最富集的盆地之一(图1(a))(Li et al., 2024; Yu et al., 2024; Xiao et al., 2024)。实验岩心采自齐家古龙凹陷(图1(b))。

松辽盆地主要发育于白垩纪,晚白垩纪发生大规模湖侵,尤其是在青山口组和嫩江组沉积时期,导致半深湖—深湖相沉积广泛分布。在青山口组,一次大规模湖侵形成了大型且稳定的湖盆(Li et al., 2024; Yu et al., 2024; Xiao et al., 2024)。根据岩性和组分特征,页岩层(一段 Q₁ 和二段下部 lower Q₂)的主要产油层段可细分为 9 个油层,总厚度为 80–130 m(图1(c))(Zhou et al., 2023)。全直径岩心取自 Q₉ 层,该层被划分为纯页岩型页岩。这些岩心层理裂缝发育,裂缝面相对平直,裂缝密度为每米 500–1000 条层理裂缝。

**图1.** 松辽盆地取心井 X 的位置与岩性:(a) 中国东北部松辽盆地;(b) 取心井 X 在齐家古龙凹陷的位置;(c) 取心井 X 中青山口组岩性(修改自 Zhao et al., 2023)。

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## 3. 研究方法

### 3.1 实验材料与方法

#### 3.1.1 材料

实验材料包括:松辽盆地青山口组取心井 X 的全直径页岩岩心(直径 × 长度 = 11 × 12 cm);硅胶模具(长 × 宽 × 高 = 10 × 10 × 10 cm);去离子水;KCl(上海阿拉丁生化科技股份有限公司,纯度 ≥ 99.98%);CTAB(上海阿拉丁生化科技股份有限公司,纯度 ≥ 99.0%);SiO₂ 纳米流体母液(中国石油大学(华东)配制,平均粒径 = 6 nm);环氧树脂胶(AB 水晶胶,按 3:1 比例混合);亚克力结构 AB 胶(德国 Kisling 公司,按 1:1 比例混合);钢管(外径 = 8 mm,内径 = 6 mm)。

#### 3.1.2 方法

**(1) 岩心样品制备**

① 将全直径岩心(图2(d))使用线切割装置切割成 9 cm × 9 cm × 9 cm 的立方体页岩岩心,并分别放入硅胶模具中。利用剩余页岩材料加工圆柱形页岩岩心(直径 × 长度 = 2.5 × 4 cm),随后通过实验室测试测量其水平空气渗透率和孔隙率。

② 将立方体页岩岩心置于 10 cm × 10 cm × 10 cm 硅胶模具中心。然后向模具中倒入环氧树脂胶并固化 24 h(图2(f))。为防止模具变形,使用亚克力板进行固定。封装后的岩心设计为可放入 10 cm × 10 cm × 10 cm 岩心夹持器中。此外,环氧树脂层可防止后续钻取和卸压过程中样品受到机械损伤。

③ 取出封装后的页岩岩心,使用 8 mm 钻头沿垂直层理方向钻一个深 4.5 cm 的圆形孔。

④ 将长 6 cm 的钢管插入孔中,并使用亚克力结构 AB 胶固定,然后固化 24 h。

⑤ 使用 6 mm 钻头从岩心上表面钻一个深 5.5 cm 的孔,完成封装和插管后的岩心制备(图2(e))。

**(2) 水力诱导裂缝扩展实验**

① 在钻取后、钢管固定前,使用 X 射线 CT 扫描仪对立方体页岩岩心进行扫描和重建。CT 扫描分辨率为 53 μm。

② 配制 0.75%(质量分数)KCl 溶液,并以该 KCl 溶液为基液,分别配制 0.1% CTAB 溶液、0.1% SiO₂ 溶液以及 0.1% CTAB 和 SiO₂ 混合溶液(CTAB : SiO₂ 纳米流体 = 1:1)。

③ 将配制好的流体注入中间容器,关闭出口端,并检查装置是否泄漏。

④ 将封装并插管后的岩心放入真三轴压裂实验装置的岩心室中,并在 x、y、z 三个方向施加 8 MPa 的恒定压力。

⑤ 以 10 mL/min 的流量向页岩岩心中注入流体,直至达到峰值压力。

⑥ 分别以 0.5、1、2、3、4、5 和 6 mL/min 的流量注入流体,每 2 min 调整一次流量,并记录注入压力。

**图2.** 实验设备与制备岩心:(a) 真三轴水力压裂实验系统;(b) nanoVoxel 3000 X 射线 CT 扫描仪(分辨率:0.5 μm);(c) D8AA25 高分辨率 X 射线衍射仪(Bruker,德国);(d) 取心井 X 的全直径岩心;(e) 水力压裂岩心制备过程;(f) 涂覆环氧树脂胶的立方体页岩岩心。

⑦ 取出岩心内部钢管,再次使用 X 射线 CT 扫描仪对岩心进行扫描和重建。使用 AVIZO 软件进行裂缝提取(Avizo, 2019)。CT 扫描按照《微束分析—致密岩石微纳孔隙结构计算机断层扫描(CT)成像方法》(GB/T 38531-2020)执行。

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### 3.2 数值模拟

#### 3.2.1 模拟方法

**(1) 控制方程**

对于黏性流体,空间中任意一点的流速(u)、压力(p)和密度(ρ)满足基于质量守恒的连续性方程:

∂ρ/∂t + ∇·(ρu) = 0 (1)

其中:

∇·(ρu) = ∂ρuₓ/∂x + ∂ρu_y/∂y + ∂ρu_z/∂z (2)

对于不可压缩流体,密度不随时间和空间变化。因此,连续性方程简化为:

∇·u = 0 (3)

设单位体积体积力为 F,单位体积表面应力为 ∇·σ。根据牛顿第二定律:

ρ Du/Dt = ρF + ∇·σ (4)

其中 σ 为总应力:

σ = −pI + τ (5)

Du/Dt 为质点加速度:

Du/Dt = ∂u/∂t + (u·∇)u (6)

对于弹性固体,变形与应力关系遵循胡克定律;对于黏性流体,则遵循斯托克斯定律:

τ = μ(∇u + ∇uᵀ) (7)

基于连续性方程和牛顿第二定律的推导,在忽略重力的假设下,可得到不可压缩流体的纳维—斯托克斯方程。裂缝内稳态流动采用纳维—斯托克斯方程求解(Panton, 2013):

{ ρ[∂u/∂t + (u·∇)u] = ∇(−pI + μ[∇u + (∇u)ᵀ]) ∇u = 0 } (8)

其中:ρ 为流体密度,kg/m³;u 为流体速度,m/s;t 为时间,s;p 为流体压力,Pa;I 为单位矩阵;μ 为流体黏度,Pa·s。

**(2) 边界条件**

各模型的边界条件如下:左侧为入口,右侧为出口,入口给定速度。出口压力设为 0,页岩表面处理为无滑移边界。

入口边界条件:

u = u₀;n·μ(∇u + (∇u)ᵀ) = 0 (9)

出口边界条件:

p = p₀;n·μ(∇u + (∇u)ᵀ) = 0 (10)

固体壁面边界:

u = 0 (11)

其中 n 为单位法向量。

#### 3.2.2 模型设计与假设

**(1) 模型设计**

模拟过程中,注入流体黏度为 1 mPa·s,密度为 1000 kg/m³。注入速度为 0.1 m/s,出口压力为 0 Pa。实验中不同流体诱导的水力裂缝使用 Avizo 软件提取(Avizo, 2019)。数值模拟时,针对每种流体选取具有代表性的局部裂缝,尺寸为 5.3 mm(长)× 3.7 mm(宽)。每个岩心中部分裂缝的边界层厚度和网格尺寸均设为 5 μm。各模拟算例的总网格数见表1。

**表1** 不同页岩岩心中部分裂缝的网格划分。

| 岩心编号 | S156 | S148 | S93 | S132 | |---|---|---|---|---| | 流体类型 | KCl 溶液 | CTAB 溶液 | SiO₂ 溶液 | CTAB 和 SiO₂ 混合溶液 | | 网格数 | 2404557 | 3625455 | 2730596 | 2077997 |

**(2) 模型假设**

本研究采用层流模型(斯托克斯流)模拟不同流体在多孔介质微裂缝中的渗流行为。为简化计算,作如下假设:

① 注入流体视为不可压缩流体。 ② 渗流过程中流体保持等温。 ③ 所有流体具有相同的密度和黏度。 ④ 由于模型尺度较小,忽略重力影响。

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## 4. 结果与讨论

### 4.1 页岩岩心的矿物组成与物理特征

页岩的矿物组成会影响其矿化反应和力学性质(Zhao et al., 2023; Zhou et al., 2023; Hong et al., 2024)。为表征本研究所用全直径页岩样品的理化性质,采用 X 射线衍射分析岩心样品的矿物组成。结果如图3(a)所示,为总体矿物组成;图3(b)为黏土矿物组成。

页岩主要由黏土矿物、石英和斜长石组成,其中黏土占 54.2%,石英占 22.6%,斜长石占 15.4%。与其他盆地页岩油藏相比,其黏土矿物和斜长石含量相对较高(Zhou et al., 2023)。黏土矿物组成以伊利石、伊利石—蒙脱石混层和绿泥石为主。伊利石含量为 59.7%,伊利石—蒙脱石混层含量为 27.1%,绿泥石含量为 9.7%。松辽盆地页岩经历了较深成岩作用,导致蒙脱石向伊利石转化,并伴随硅质沉淀,从而增强了页岩的刚性和脆性(Sun et al., 2021)。

全直径页岩岩心的孔隙率为 3.7%–4.2%,平均为 4.0%(图3(c))。水平渗透率为 0.011 × 10⁻³–0.015 × 10⁻³ μm²,平均为 0.013 × 10⁻³ μm²(图3(d))。这些孔隙率和渗透率值表明储层物性较差。宏观观察发现,页岩表面存在大量层理裂缝,这些天然裂缝可能有利于流体沿其侵入(Sun et al., 2023; Shi et al., 2023)。

**图3.** 矿物组成与孔隙率—渗透率特征:(a) 岩心 S148 的矿物含量;(b) S148 的黏土矿物含量;(c) 不同全直径岩心的渗透率;(d) 不同全直径岩心的孔隙率。

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### 4.2 水力诱导裂缝实验

注入压力曲线的变化特征对于理解页岩中水力裂缝扩展至关重要(Yang et al., 2022, 2023; Li et al., 2023)。不同流体在全直径页岩岩心中诱导水力裂缝的压力—时间曲线如图4所示。

注入 KCl 溶液时,注入压力达到 61.1 MPa,沿层理面诱导水力压裂,随后急剧下降至 12.9 MPa(图4(a))。注入 CTAB 溶液时,注入压力达到 43.9 MPa,沿层理面诱导水力压裂,随后注入压力迅速下降至 4.5 MPa(图4(b))。注入 SiO₂ 溶液时,注入压力达到 30.5 MPa,沿层理面诱导水力压裂,随后迅速下降至 3.3 MPa(图4(c))。注入 CTAB 和 SiO₂ 混合溶液时,注入压力达到 57.3 MPa,沿层理面诱导水力压裂,随后急剧下降至 11.1 MPa(图4(d))。

一般地,当注入压力低于破裂压力时,流体充满井筒并发生井筒储存和压缩,导致压力逐渐升高。一旦达到层理起裂压力,胶结较弱的页岩层理面被激活。随后,流体沿诱导裂缝从井筒快速突破,向岩心边缘流动并流出,导致注入压力急剧下降。值得注意的是,不同流体通过水化作用在全直径页岩岩心中诱导裂缝起裂所需的峰值压力存在显著差异。这些差异可归因于不同流体引起的水化程度差异以及内部层理裂缝的原有损伤。此外,在 CTAB 溶液和 SiO₂ 溶液诱导全直径页岩岩心水力裂缝扩展后,注入压力受施加的三轴压应力影响,并低于三轴应力。这表明岩心内部发生了破碎,页岩碎屑支撑裂缝壁面,防止新诱导裂缝闭合,从而提高了岩心的导流能力。

**图4.** 不同流体的注入压力—时间关系:(a) 岩心 S156 注入 KCl 溶液;(b) 岩心 S148 注入 CTAB 溶液;(c) 岩心 S93 注入 SiO₂ 溶液;(d) 岩心 S132 注入 CTAB 和 SiO₂ 混合溶液。

在不同流体诱导全直径页岩岩心形成水力裂缝后,随后以递增速率注入各流体。注入速率每 2 min 增加一级,并以 1 s 间隔记录每种流体的压力—时间关系(图5)。实验过程中诱导的水力裂缝贯穿全直径岩心并延伸至岩心表面,裂缝尖端处流体压力为大气压。全直径岩心承受 8 MPa 的恒定三轴应力。注入压力反映了页岩岩心内诱导裂缝的导流能力。

注入 KCl 溶液时,当注入速率增至 5 mL/min,注入压力 initially 上升。然而,在 3 和 5 mL/min 注入速率下均观察到显著压力下降(图5(a))。当注入速率达到 6 mL/min 时,注入压力发生急剧下降。这表明在 KCl 溶液注入过程中,水化和侵蚀作用导致岩心裂缝优势渗流通道内较大的层状页岩碎屑剥落和迁移。这些页岩碎屑支撑了开启裂缝内的优势渗流通道,并提高了其导流能力。

注入 CTAB 溶液时,将注入速率增至 6 mL/min,所有测试速率下注入压力均上升,同时保持相对稳定的导流能力(图5(b))。这表明 CTAB 溶液注入形成的水力诱导裂缝内部结构稳定,被侵蚀、剥落和运移的页岩碎屑支撑局部开启裂缝,使导流能力更加稳定。

注入 SiO₂ 溶液时,将注入速率增至 6 mL/min,裂缝导流能力相对稳定,与 CTAB 溶液注入时观察到的情况相似(图5(c))。这表明与 KCl 溶液相比,CTAB 溶液和 SiO₂ 溶液进一步抑制了页岩表面水化,使裂缝接触面具有更稳定的力学性质。一些研究表明,水化可显著降低页岩表面稳定性和力学性质(Cui et al., 2023; Hong et al., 2024)。然而,CTAB 和 SiO₂ 均可促进黏土层间距收缩,增强黏土矿物晶体稳定性,并保持其力学性能,从而抑制黏土矿物内部水分子运移(Shi et al., 2023; Karimi et al., 2023)。

注入 CTAB 和 SiO₂ 混合溶液时,将注入速率增至 2 和 4 mL/min,后期出现显著压力下降(图5(d))。然而,在 3 和 5 mL/min 注入速率下,注入压力持续上升。当注入速率达到 6 mL/min 时,随着注入量增加,压力先下降后上升。这表明在 CTAB 和 SiO₂ 混合溶液注入过程中,流体持续侵蚀并运移页岩岩心内剥落的小颗粒黏土或石英。这些被动员的颗粒随后迁移至流道中,积聚并最终堵塞流道。

当流道内注入压力逐渐升高到某一阈值时,被堵塞的流道被冲开。这导致岩心内导流能力先增大后减小的过程。因此,溶液中 CTAB 和 SiO₂ 的强耦合作用过度抑制了页岩水化,影响了页岩碎屑的剥落。结果是,开启裂缝难以得到有效支撑,更容易闭合。

对不同流体诱导水力裂缝内最终导流能力的综合比较表明,其顺序为:SiO₂ 溶液(S93)> CTAB 溶液(S148)> KCl 溶液(S156)> CTAB 和 SiO₂ 混合溶液(S132)。

**图5.** 全直径岩心中不同流体起裂后的注入压力—时间关系:(a) KCl 溶液岩心 S156;(b) CTAB 溶液岩心 S148;(c) SiO₂ 溶液岩心 S93;(d) CTAB 和 SiO₂ 混合溶液岩心 S132。

为研究不同流体诱导的实际裂缝扩展,对经历水力裂缝扩展的全直径页岩岩心进行 CT 扫描,以比较压裂前后状态。页岩岩心重建表面状态如图6所示。从岩心重建图像可观察到,注入 KCl 溶液后,岩心前端形成一条明显裂缝。该现象可通过区域 I(图6(a))与区域 II(图6(b))的对比观察到。相比之下,注入 CTAB 溶液后,岩心前端形成三条清晰裂缝。该现象可通过区域 III(图6(c))与区域 V(图6(d))以及区域 IV(图6(c))与区域 VI(图6(d))的对比观察到。注入 SiO₂ 溶液和 CTAB 和 SiO₂ 混合溶液后,岩心前端未观察到明显裂缝。这表明全直径页岩岩心在层理方向上具有显著非均质性,流体穿透位置在岩心范围内无明显规律。然而值得注意的是,KCl 溶液和 CTAB 溶液诱导的裂缝与层理面平行。

**图6.** 不同流体在全直径岩心中诱导水力裂缝的三维重建图像:(a) 岩心 S156 注入 KCl 溶液前;(b) 岩心 S156 注入 KCl 溶液后;(c) 岩心 S148 注入 CTAB 溶液前;(d) 岩心 S148 注入 CTAB 溶液后;(e) 岩心 S93 注入 SiO₂ 溶液前;(f) 岩心 S93 注入 SiO₂ 溶液后;(g) 岩心 S132 注入 CTAB 和 SiO₂ 混合溶液前;(h) 岩心 S132 注入 CTAB 和 SiO₂ 混合溶液后。

为进一步研究不同流体诱导水力裂缝的形态,采用亮度分割方法提取裂缝网络(Zhang et al., 2024b)。不同流体诱导的页岩岩心中裂缝分布结果如图7所示。研究发现,KCl 溶液、SiO₂ 溶液以及 CTAB 和 SiO₂ 混合溶液诱导的水力裂缝仅沿单一层理方向扩展(图7(a–e) 和 (g))。所形成裂缝相对光滑,裂缝轨迹无明显变化。相比之下,CTAB 溶液诱导的水力裂缝沿层理面在不同水平位置形成三条明显裂缝(图7(c))。诱导裂缝仅向一个方向延伸,未观察到对侧激活。随着距注入点距离增加,裂缝开度增大。这进一步表明,注入点附近被侵蚀的页岩碎屑或小颗粒被运移至更远处,支撑局部裂缝,使这些裂缝开度增大,从而提高其导流能力。该现象在每种流体诱导的局部裂缝放大图像中清晰可见。这些裂缝代表局部连通性,形成复杂渗流区域。然而,这些区域内的流动模式不规则,沿裂缝不同位置的渗流行为仍难以预测。

**图7.** 不同流体注入后诱导的水力裂缝:(a) 岩心 S156 注入 KCl 溶液后;(b) (a) 的局部放大;(c) 岩心 S148 注入 CTAB 溶液后;(d) (c) 的局部放大;(e) 岩心 S93 注入 SiO₂ 溶液后;(f) (e) 的局部放大;(g) 岩心 S132 注入 CTAB 和 SiO₂ 混合溶液后;(h) (g) 的局部放大。

在不同流体对全直径岩心进行水力压裂后,观察上下裂缝表面发现,局部位置存在层状页岩碎屑。这些页岩碎屑在区域 I–V(图8(a–e))中被观察到。这些页岩碎屑在页岩岩心内构成自支撑渗流系统。研究发现,CTAB 溶液水力效应诱导的裂缝不仅沿水平层理面扩展,还在垂向表现出局部书页状裂缝。该现象在图8(g) 的区域 VI 中被观察到。这种复杂裂缝模式不仅导致页岩碎屑支撑裂缝(图8(k)),还在岩心内形成滑撑裂缝(图8(i)),显著增强了裂缝的各向异性导流能力。此外,裂缝表面碎屑剥落区域形成潜在优势渗流通道,从而进一步提高导流能力。相比之下,CTAB 和 SiO₂ 混合溶液诱导的裂缝表面相对平整光滑,使小颗粒支撑裂缝的上下裂缝表面匹配性更好。这些平整光滑的裂缝表面在围压下容易闭合(图8(e)),显著降低导流能力。值得注意的是,在裂缝表面观察到大量小颗粒,进一步证实颗粒迁移和积聚循环导致不同速率注入过程中导流能力显著波动(图8(l))。

**图8.** 不同流体注入后全直径岩心中的裂缝表面与支撑模式:(a) KCl 溶液注入后上表面;(b) KCl 溶液注入后下表面;(c) CTAB 溶液注入后上表面;(d) CTAB 溶液注入后下表面;(e) SiO₂ 溶液注入后上表面;(f) SiO₂ 溶液注入后下表面;(g) CTAB 和 SiO₂ 混合溶液注入后上表面;(h) CTAB 和 SiO₂ 混合溶液注入后下表面;(i) 闭合裂缝;(j) 滑移裂缝;(k) 碎屑支撑裂缝;(l) 颗粒支撑裂缝。

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### 4.3 水力诱导裂缝中渗流模拟

不同流体在全直径页岩岩心中诱导的局部裂缝速度场如图9所示。这些裂缝对应图7中所示的局部水力诱导裂缝。研究发现,KCl 溶液和 CTAB 溶液诱导的局部裂缝流道由树枝状结构逐渐汇聚为统一渗流区,其导流能力逐步增加(图9(a–d))。这是由于统一渗流区周围页岩碎屑的支撑作用,而较远处裂缝倾向于分散闭合。SiO₂ 溶液诱导的局部裂缝流道由一种分散树枝状结构演变为另一种分散树枝状结构。该行为发生的原因是页岩碎屑在裂缝中段提供结构支撑,而随着距这些碎屑距离增加,裂缝逐渐分散闭合。

在 CTAB 和 SiO₂ 混合溶液诱导的局部裂缝中,仅在中部和边缘存在狭窄流道,严重限制了这些裂缝中的流体流动。该现象在图9(d) 的区域 VII 中被观察到。与主流道相比,局部接触面附近较窄流道中的流速显著更高。该现象在区域 I(图9(a))、区域 III(图9(b))以及区域 V 和 VI(图9(c))中被观察到。随着流道变宽,局部区域流速呈径向降低,流体逐渐汇聚到较大流道中(图9(f))。该现象主要归因于这些局部裂缝区缺乏页岩碎屑支撑。值得注意的是,在 KCl 溶液、SiO₂ 溶液和 CTAB 和 SiO₂ 混合溶液诱导的局部裂缝盲端,几乎没有流体运动,这些区域内流体呈滞止状态。该现象在区域 II(图9(a))和区域 VIII(图9(d))中被观察到。

**图9.** 不同流体诱导的局部三维裂缝速度场:(a) KCl 溶液;(b) CTAB 溶液;(c) SiO₂ 溶液;(d) CTAB 和 SiO₂ 混合溶液;(e) (c) 中 V 的放大图;(f) (b) 中 VI 的放大图。

通过数值模拟获得不同流体在全直径页岩岩心中诱导的局部裂缝压力场和流线场(图10)。结果表明,不同流体在页岩裂缝中的压力分布和流动行为存在显著差异。

研究发现,KCl 溶液诱导的局部裂缝在左上区域较窄流道中表现出较高注入压力。注入流体以树枝状模式向中心区域汇聚,随后又以分支流动形式再次分散,裂缝网络内观察到相对平缓的压力梯度(图10(a))。这可归因于页岩碎屑支撑的局部裂缝开度相对均匀,有利于流体顺畅流动。

相比之下,CTAB 溶液在裂缝右下区域形成局部树枝状流道(图10(b))。在相同注入速率条件下,当流道变窄时,压力梯度出现显著变化(图10(e))。该现象源于该位置强烈裂缝闭合,使流道收缩,进而导致压力梯度剧烈变化。

SiO₂ 溶液在局部裂缝中表现出最平缓的压力梯度(图10(c)),表明页岩碎屑在该位置对裂缝形成均匀支撑,使流体以稳定压力梯度流动。这种均匀自支撑作用有效防止裂缝闭合,从而保持较高导流能力。

CTAB 和 SiO₂ 混合溶液仅在中心裂缝区边缘形成一条次要流道(图10(f)),导致注入压力在该位置集中。该现象在图10(d) 的区域 II 中被观察到。流体通过该狭窄段后,注入压力迅速降低,并呈径向扩散模式。该现象在图10(d) 的区域 II 中被观察到。这表明该位置局部裂缝缺乏页岩碎屑内部支撑,而优势渗流通道内细颗粒积聚严重阻碍流体运动。

**图10.** 不同流体诱导的局部三维裂缝压力场与流线场:(a) KCl 溶液;(b) CTAB 溶液;(c) SiO₂ 溶液;(d) CTAB 和 SiO₂ 混合溶液;(e) (b) 中 I 的放大图;(f) (d) 中 II 的放大图。

为定量研究不同流体诱导水力裂缝中注入速率与压差之间的关系,分析了不同注入速率下局部裂缝注入端与出口端之间压差的变化。研究发现,在每个岩心的局部裂缝中,压差随注入速率增加而逐渐增大,且增长速率也变得更加显著。在相同注入压力下,SiO₂ 溶液诱导的裂缝表现出最高导流能力。KCl 溶液和 CTAB 溶液诱导的局部裂缝导流能力相对接近。值得注意的是,在低流速(u < 0.3 m/s)下,KCl 溶液诱导的裂缝表现出更高导流能力。然而,当流速超过 0.3 m/s 时,CTAB 溶液诱导裂缝的导流能力逐渐超过 KCl 溶液诱导裂缝的导流能力。

CTAB 和 SiO₂ 混合溶液诱导的局部裂缝表现出最低导流能力(图11(a))。模拟结果表明,各流体诱导局部裂缝的导流能力顺序为:SiO₂ 溶液(S93)> CTAB 溶液(S148)和 KCl 溶液(S156)> CTAB 和 SiO₂ 混合溶液(S132),这与实验结果一致(图11(b))。

**图11.** (a) 不同流体的注入压力—速度关系;(b) 0.4 m/s 下的注入压力。

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### 4.4 讨论

松辽盆地陆相页岩以层理发育为特征(也称为层理裂缝),这代表了页岩水化前固有的微损伤。对于具有初始损伤的岩土结构,流体注入可在这些已有损伤部位诱导新的微损伤。随着微损伤不断累积,逐渐演化为宏观裂缝,最终形成有效裂缝渗流系统。此外,页岩层理面和剖面的微观结构对页岩导流能力也有显著影响。

在极低渗透率陆相页岩油藏中,孔隙尺寸通常处于纳米尺度。此外,松辽盆地页岩通常为油湿油藏(Sun et al., 2021; Zhang et al., 2023a, 2023b),导致页岩基质水渗吸能力差,进而抑制注入流体在页岩基质中的流动。CTAB 和 SiO₂ 纳米颗粒对黏土矿物起保护作用,降低水化效应,使破碎页岩碎屑不易膨胀和崩解。这种稳定作用有助于保持更一致的导流能力。此外,流体水力诱导形成的裂缝逐渐成为页岩油从基质孔隙流向井筒的关键通道。

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## 5. 结论

本研究针对中国松辽盆地全直径页岩岩心,研究了不同流体诱导裂缝的导流能力,并明确了注入流体在水力诱导裂缝中的渗流行为。主要结论如下:

(1) 不同流体注入可沿页岩层理面诱导裂缝开启,形成有效渗流系统。裂缝表面相对平整光滑,未观察到明显裂缝转向。

(2) 注入端附近被侵蚀和剥落的页岩碎屑被运移至更远处,并对裂缝起支撑作用。这些位置裂缝开度增大,导流能力提高。该行为与常规水力压裂中观察到的行为不同。

(3) CTAB 溶液和 SiO₂ 溶液均降低了页岩表面水化程度,稳定了裂缝界面力学性质。因此,页岩碎屑不易膨胀和崩解,导流能力更加稳定。

(4) CTAB 溶液和 SiO₂ 溶液诱导的裂缝导流能力均高于 CTAB 和 SiO₂ 混合溶液诱导的裂缝导流能力。混合溶液的耦合作用强烈抑制页岩水化,使页岩碎屑不易剥落,从而无法有效支撑裂缝开度。

(5) KCl 溶液、SiO₂ 溶液和 CTAB 和 SiO₂ 混合溶液注入诱导的水力裂缝均仅沿优势页岩层理面形成单一裂缝。相比之下,CTAB 溶液沿页岩层理面在不同水平位置诱导形成三条明显裂缝。

(6) 随着距页岩碎屑空间距离增加,裂缝逐渐呈现分散闭合。闭合区附近较小流道中的流速明显高于主流道中的流速,导致显著绕流现象。这阻碍了流体通过页岩岩心的有效渗流。

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## CRediT 作者贡献声明

**Hong-Tao Fu:** 撰写—初稿、方法、研究、概念化。 **Kao-Ping Song:** 撰写—审阅与编辑、监督、资源、经费获取。 **Er-Long Yang:** 软件、资源、研究。 **Yu Zhao:** 资源、经费获取、形式分析。 **Xi Xia:** 可视化、监督、软件、概念化。 **Li-Hao Liang:** 撰写—审阅与编辑、方法、形式分析。

## 数据可用性声明

支持本研究结果的数据可向通讯作者合理请求获取。

## 利益冲突声明

作者声明不存在利益冲突。

## 致谢

本研究得到以下项目资助:高温高盐 offshore 油田间断式与变圈模式活性纳米流体驱提高采收率前沿与基础研究(U22B6005);国家自然科学基金(No. 52274037);古龙页岩油提高采收率关键问题研究(DQYT-2022-JS-761)。

## 附录 A. 补充数据

本文补充数据可在线获取:https://doi.org/10.1016/j.petsci.2025.09.035。