In situ X-ray micro-CT for investigation of damage evolution in black shale under uniaxial compression

Crack damage evolution of shale is crucial to the hydraulic fracturing treatment and engineering stability. Although many effects have been done on the macroscopic characteristics of shale, yet the microscopic failure mechanism is not well understood. A uniaxial compressive test on black shale was conducted under topographic monitoring using in situ X-ray micro-tomography (µCT). A series of high-resolution reconstruction images were obtained by carrying out CT scans at six key points throughout the test to obtain the internal structure of shale sample. In addition, the CT values for the purpose of crack damage evolution in shale were identified. Clear 2D/3D CT images, CT value analysis and image segmentation analysis reveal that the sample experiences compression, damage, cracking, crack propagation, and collapse stages. Crack geometry and distribution in the shale sample is visualized by rendered CT images, and a combined tension and shear failure mode is observed from the fracture rose diagram. This work suggests that formation and propagation of fractures are influenced by the stratified structure and weak cementation medium between layers.     

基于核磁共振的脆硬性泥页岩水化损伤演化研究

为研究脆硬性泥页岩水化后细观结构的损伤演化特征,利用核磁共振技术对不同浸泡时间的脆硬性泥页岩试样进行测量,得到不同浸泡时间的试样质量变化、横向弛豫时间T2谱分布以及核磁共振成像。结果表明：水化作用会对岩石内部产生损伤,岩样吸水率在最初的8 h内变化相对较大,1 d后相对接近稳定,之后变化不明显。随着浸泡时间的延长,微裂缝在水化的作用下快速扩展、贯通使岩样表面产生明显裂纹。核磁共振T2谱图和成像结果表明,水化作用使岩样微观结构重新分布,T2曲线信号幅度发生明显的变化,并随着浸泡时间的延长而增加。整个水化损伤分为3个阶段：大尺寸孔隙裂纹发展阶段;小孔隙产生、大尺寸孔隙裂纹加剧扩展;小孔隙加剧产生扩展、大尺寸孔隙裂纹归并贯通至水化破坏阶段。核磁共振图像显示同一块岩样在不同浸泡时间的内部微观结构分布,动态地显示岩石的水化损伤过程。     

Nanochemomechanical assessment of shale: a coupled WDS-indentation analysis

Establishing the links between the composition, microstructure and mechanics of shale continues to be a formidable challenge for the geomechanics community. In this study, a robust methodology is implemented to access the in situ chemomechanics of this sedimentary rock at micrometer length scales. Massive grids of coupled wave dispersive spectroscopy (WDS) and instrumented indentation experiments were performed over representative material surfaces to accommodate the highly heterogeneous composition and microstructure of shale. The extensive datasets of compositional and mechanical properties were analyzed using multi-variate clustering statistics to determine the attributes of active phases present in shale at microscales. Our chemomechanical analysis confirmed that the porous clay (PC) mechanical phase inferred by statistical indentation corresponds to the clay mineral phase defined strictly on chemical grounds. The characteristic stiffness and hardness behaviors of the PC are realized spatially in regions removed from silt inclusions of quartz and feldspar. At the microscale shared by indentation and WDS experiments, a consistent chemomechanical signature for shale emerges in which the heterogeneities of the PC are captured by the standard deviations of indentation properties and concentrations of chemical elements. However, these local behaviors are of second order compared to the global trend observed for mean mechanical properties and the clay packing density, which synthesizes the relative volumes of clay and nanoporosity in the material. The coupled statistical indentation and WDS technique represents a viable approach to characterize the chemomechanics of shale and other natural porous composites at a consistent scale below the macroscopic level.     

基于宽频大地电磁法的页岩气探测实践——以川西南沐川地区须家河组为例

四川盆地上三叠统须家河组陆相富有机质页岩较为发育,页岩连续厚度较大,含气性好,有望开辟四川盆地页岩气新区新层系。然而,复杂的人文干扰（城镇密集、人口众多）和较大的埋藏深度（2000~3000m）挑战了页岩气地球物理勘探的精度,这在很大程度上制约了川西南沐川地区三叠系须家河组页岩气的进一步勘探。本文在分析前人研究资料基础上,优选了川西南沐川地区须家河组作为新区新层系的探测目标,根据研究区地质情况,构建理论电性模型,通过正演模拟和“已知”钻孔标定方法试验,确定了宽频大地电磁法的适用性和有效性。进而在重点页岩气远景区部署一条宽频大地电磁剖面,通过数据处理分析,结合地质资料获得了研究区深部电性结构,认为研究区一带地层连续、完整,断裂不发育,具有稳定的地质结构,其中上三叠统须家河组发育较大厚度的富有机质页岩,可作为本区页岩气勘探的新区新层系,具有良好的页岩气、致密气资源前景。同时,证实了在3000m以浅页岩气探测方法中,宽频大地电磁法（BMT）可以有效地识别富有机质页岩规模和空间展布特征,是一种快速、经济、无损有效的页岩气探测方法,可以为页岩气勘探提供先导依据,同时也为同类地质情况页岩气探测提供应用示范。     

Microstructure Evolution of Organic Matter and Clay Minerals in Shales with Increasing Thermal Maturity

As the two important components of shale, organic matter(OM) and clay minerals are usually thought to strongly influence the hydrocarbon generation, enrichment and exploitation. The evolution process of OM and clay minerals as well as their interrelationship over a wide range of thermal maturities are not completely clear. Taking Yanchang(T_3y), Longmaxi(S_1l) and Niutitang(?_1n) shales as examples, we have studied the microstructure characteristics of OM and clay minerals in shales with different thermal maturities. The effects of clay minerals and OM on pores were reinforced through sedimentation experiments. Using a combination of field emission scanning electron microscopy(FESEM) and low-pressure N_2 adsorption, we investigated the microstructure differences among the three shales. The results showed that both OM and clay minerals have strong effects on pores, and small mesopore(2–20 nm) is the dominant pore component for all three samples. However, the differences between the three samples are embodied in the distribution of pore size and the location. For the T_3y shale, clay minerals are loosely arranged and develop large amounts of pores, and fine OM grains often fill in intergranular minerals or fractures. Widespread OM pores distribute irregularly in S_1l shale, and most of the pores are elliptical and nondirectional. The ?_1n shale is characterized by the preferred orientational OM-clay aggregates, and lots of pores in the composites are in the mesopore range, suggesting that over maturity lead to the collapse and compaction of pores under huge pressure of strata. The results of the current research imply that with increasing thermal maturity, OM pores are absent at low maturity(T_3y), are maximized at high maturity(S_1l) and are destroyed or compacted at over-mature stage(?_1n). Meanwhile, clay minerals have gone through mineral transformation and orientational evolution. The interaction of the two processes makes a significant difference to the microstructure evolution of OM and clay minerals in shale, and the findings provide scientific foundation in better understanding diagenetic evolution and hydrocarbon generation of shale.     

The granular and polymer composite nature of kerogen-rich shale

In the past decade, mechanical, physical, and chemical characterization of reservoir shale rocks, such as the Woodford shale, which is kerogen-rich shale (KRS), has moved toward micro- and nanoscale testing and analyses. Nanoindentation equipment is now widely used in many industrial and university laboratories to measure shale anisotropic Young’s moduli, kerogen stiffness, plastic yield parameters, and other isotropic and anisotropic poromechanical and viscoelastic properties. However, to date, failure analyses of KRS and the effects of organic components on the tensile strength have not been observed or measured at the micro- or nanoscales. In this study, preserved kerogen-rich Woodford shale samples manufactured in micro-beam and micro-pillar geometries were mechanically tested and brought to failure in tension and compression, respectively. These tests were conducted in situ using a nanoindenter inside a scanning electron microscope (SEM). The load versus displacement curves of prismatic micro-cantilever beams were analyzed in light of high-resolution images collected during tensile fracture initiation, propagation, and ultimately sample failure. The micro-pillar geometries were subjected to a uniaxial compressive load and were also brought to failure while capturing measurements of stress and strain. It was found that, within just a few hundred microns of the KRS micro-cantilever beams, both brittle and ductile failure modes were observed. In the ductile plastic domain, strain-softening and strain-hardening behaviors were identified and characterized. These were not due to confining stress variations, but due to the volume of the organic matter and the way it is interlaced with the shale minerals in and around the failure planes. The tensile strength characteristics and the large modulus of toughness of kerogen, which is a cross-linked polymer, definitely weigh heavily in our engineering field applications, such as hydraulic fracking, which is a Mode I tensile fracture opening and propagation phenomenon. This practice demands that, due to the complex composite nature of KRS, mechanical characterization be not only for unconfined compressive strength but also for unconfined tensile strength and moduli of ruptures. At the end of this study, the need for nanometer scale mechanical characterization of KRS will become apparent. These nano- and micro-scale shale failure tests reinforce our previous understanding of the heterogeneous composite nature of Woodford KRS and its complex behavior, as well as other source shale reservoir formations.     

Quantitative analysis of meso-damage evolution for shale under in situ uniaxial compression conditions

In order to investigate the meso-damage evolution of shale, four uniaxial compressive tests were conducted using X-ray micro-computed tomography (micro-CT) equipment. Two of the four samples were conducted the in situ compression tests, from which a series of CT images at different stress levels were got during the loading process. Based on those CT images, a new damage variable was first proposed to quantitatively analyze the damage evolution of shale under uniaxial compression condition. Analysis results show that the evolution of the damage variable is consistent with both the mesoscopic CT images and the macroscopic stress–strain, which can well characterize the meso-damage evolution of shale. Additionally, the parameters of crack area and crack length were obtained to quantitatively describe the cracking characteristics. The statistical results demonstrate that the distributions of crack are closely related to the scanning stress levels and the scanning elevations. These quantitative conclusions are important to understand the meso-damage evolution and the cracking mechanism of shale.     

应用时间序列InSAR技术监测上海磁悬浮列车专线形变

新代高分辨军、短重访周期SAR卫星的发射运行,使得InSAR技术不仅能满足大范围地表沉降监测的数据需求,还可以监测到大型人工线状地物的形变,使得对短周期微小形变的监测和预警成为可能。本文以上海市在运营的磁悬浮列车专线为研究对象,利用时间序列分析方法对20112~F9月～2012年10月期间的15景TenaSAR-X数据进行了处理和分析,实验结果表明高分辨军SAR数据可以用于公共交通设施微小形变的监测,在公共安全领域具有广阔的应用前景。     

基于计算机X射线断层术与扫描电镜图像的黄土微结构定量分析

以湿陷性黄土的电镜扫描（SEM）和三轴CT扫描试验为基础,针对CT图像分辨率较低、难以实现土微结构精确量化的缺陷,通过对不同放大倍数的SEM图像进行图像分析,并从其中选择标准训练样本,利用训练样本对CT图像进行监督分类,从而达到定量化分析土的微结构的目的。通过比较CT图像基于自身灰度分级和基于SEM训练样本两种不同方法进行监督分类,结果表明基于SEM训练样本的CT图像监督分类,可以更好地量化监测黄土大孔隙、团粒、黏土集粒和矿物颗粒在固结剪切过程中的变化规律,从而为土的微结构研究提供了新的视角。     

离子稳定剂ENI对湘西北页岩气储层护壁机理的初探

为研究一种离子稳定剂"ENI"对页岩气储层的护壁机理,以湘西北下寒武统牛蹄塘组炭质页岩为研究对象,通过抑制膨润土造浆试验、抑制页岩膨胀试验和抑制页岩分散试验,对比评价ENI作为钻井液关键处理剂的抑制性;通过扫描电镜试验考察ENI对炭质页岩细微结构的作用。试验表明:清水中加ENI后,膨润土造浆率降低52.41%,滚动回收率明显提高;提出的钻井液体系中,ENI钻井液作用下的页岩膨胀率最低,而滚动回收率最高,大于80%;同时,ENI生成的物质能填充孔隙,增强页岩颗粒间的连接。与所选用的其他处理剂相比,ENI具有更好的抑制炭质页岩水化膨胀、分散的效果,有助于维护井壁稳定。      

Geochemical environment of Cenomanian - Turonian black shale deposition at Wunstorf (northern Germany)

Major- and minor- element determinations were carried out on a high-resolution sample set obtained from a sediment drill core at Wunstorf (N. Germany). This study interval includes the black shale-bearing Hesseltal Formation associated with the Oceanic Anoxic Event 2 (OAE 2), also referred to as Cenomanian-Turonian Boundary Event (CTBE). Seven black shale packages, each containing several black shale layers, were defined by elevated TOC values, with black shale packages 1-4 deposited during OAE 2. Packages 5-7 extend above the level of the positive carbon-isotope excursion defining OAE 2, indicating that conditions favouring organic carbon burial must have prevailed longer in the Wunstorf Basin than elsewhere. Geochemical analyses revealed no significant differences between black shale packages deposited during and after OAE 2. Enrichment patterns of sulphur, iron and redox-sensitive and sulphide-forming trace metals point to suboxic to anoxic conditions existing at the sediment-water interface during black shale deposition, whereas sulphidic conditions prevailed deeper in the sediment. Variations in element/Al ratios follow cyclic patterns which are interpreted to represent climatically-induced changes in sediment supply. Reduced vertical mixing led to water-column stratification and caused black shale deposition.     

Nanochemo-mechanical signature of organic-rich shales: a coupled indentation–EDX analysis

The organic–inorganic nature of organic-rich source rocks poses several challenges for the development of functional relations that link mechanical properties with geochemical composition. With this focus in mind, we herein propose a method that enables chemo-mechanical characterization of this highly heterogeneous source rock at the micron and submicron length scale through a statistical analysis of a large array of energy-dispersive X-ray spectroscopy (EDX) data coupled with nanoindentation data. The ability to include elemental composition to the indentation probe via EDX is shown to provide a means to identify pure material phases, mixture phases, and interfaces between different phases. Employed over a large array, the statistical clustering of this set of chemo-mechanical data provides access to the properties of the fundamental building blocks of clay-dominated organic-rich source rocks. The versatility of the approach is illustrated through the application to a large number of source rocks of different origin, chemical composition, and organic content. We find that the identified properties exhibit a unique scaling relation between stiffness and hardness. This suggests that organic-rich shale properties can be reduced to their elementary constituents, with several implications for the development of predictive functional relations between chemical composition and mechanical properties of organic-rich source rocks such as the intimate interplay between clay-packing, organic maturity, and mechanical properties of porous clay/organic phase.     

黔铜地1井钻井技术及页岩气含气性分析

黔铜地1井是部署在黔东北铜仁地区铜仁向斜的一口页岩气地质调查井。本文简要阐述了该井的钻探、测井、气测录井施工技术,并通过钻探取心、地质编录、气测录井、测井、现场解析等工作手段,验证了铜仁地区区域岩石地层单位,获取了黔东北铜仁地区牛蹄塘组黑色页岩发育特征、含气性特征等第一手地质参数。分析认为牛蹄塘组海相页岩在黔东北铜仁地区分布广泛,沉积稳定,是黔铜地1井的主要含气层,整体上含气量随深度的增大而增加,气测全烃最高4%、现场解析在岩心破碎段出气量＞2600 mL、现场含气量最高达1.97 m3/t,显示了良好的保存条件和含气性,证实了铜仁地区页岩气勘探开发具有良好的前景。     

A review and research on comprehensive characterization of microscopic shale gas reservoir space

In this paper, substantial domestic and foreign research results of microscopic shale reservoir space were systemically reviewed, the research history consisting of simple observation and qualitative classification, quantitative research, the combination of qualitative and quantitative research successively as well as the characteristics of each research stage were summarized. In addition, the current problems existing in the characterization methods of shale reservoir space were also analyzed. Furthermore, based on massive actual detection of typical core samples obtained from more than 50 global shale gas wells and relevant practical experience, a comprehensive characterization method of combining qualitative with the semi-quantitative characterization was put forward. In detail, the indicators of the qualitative characterization include pore combination type and organic-matter microscopic morphology type, while the core elements of the semi-quantitative characterization include the percentage of the organic-matter area and the plane porosity of the pores of different types. Based on the reference of the naming and classification of rocks, the three-end-member diagram method was used to characterize microscopic shale reservoir space. This is achieved by plotting the three end-member diagram of 3 kinds of first-order critical reservoir spaces, i.e., organic-matter pores, matrix pores, and micro-fractures, in order to intuitively present the features of the microscopic pore combination. Meanwhile, statistic histograms of organic-matter microscopic morphology type and the plane porosity of different types of pores were adopted to characterize the development degree of second-order pores quantitatively. By this comprehensive characterization method, the importance of both pore combination and the microscopic morphology of organic matter were emphasized, revealing the control of organic-matter microscopic morphology over the organic-matter pores. What is more, high-resolution FE-SEM was adopted to obtain semi-quantitative statistics results. In this way, the features of pore development and pore combination were quantified, not only reflecting the types and storage capacity of the microscopic shale reservoir space, but also presenting the hydrocarbon-generating potential of organic matter in shale. Therefore, the results of this research are capable of providing in-depth microscopic information for the assessment and exploration and development of shale gas resources.     

层序地层格架及其对页岩储层发育特征的影响-以四川盆地龙马溪组页岩为例

为研究海相页岩沉积层序及其对页岩储层发育特征的控制作用,通过露头、岩芯研究及地化测试、有机质测试、矿物组分测试、孔隙发育特征测试等室内分析测试,结合测井小波分析,综合建立四川盆地龙马溪组的层序地层格架,并结合储层发育特征探讨层序与储层发育特征的关系。研究表明:研究区龙马溪组发育有两个三级层序;结合多口钻孔通过测井小波分析构建了研究区的高分辨率层序地层格架,识别出四个中期旋回A~D;对比各旋回内的储层发育特征,旋回A储层岩石学特征与旋回B~D存在显著差异,表现为储层有机质含量更高、水平层理更为发育、脆性矿物含量更高、微观储集空间（微—纳米级孔隙与微裂隙）发育程度更好,显示了层序旋回与储层物质成分、结构、力学脆性、含气性特征的显著相关关系,说明层序旋回是储层物性与含气性等发育特征的重要影响因素。基于前述研究,讨论了层序地层格架对储层发育的控制机理,层序格架下各旋回内沉积环境与沉积条件的差异导致储层沉积构造、物质成分与分布的差异,进而影响储层物性与含气性等特征;沉积盆地内高分辨率层序格架的建立可以为储层对比、评价与资源预测提供时间框架。建立了通过测井小波分析高分辨率层序地层格架进行储层分析对比的新方法,提出了基于储层小层分析建立页岩储层精细评价的新工作流程,有助于减少人为因素干扰,可以为页岩优质储层成因研究及其预测评价提供科学依据与新思路。     

Stepwise pyrolysis-gas chromatography of kerogen in sedimentary rocks

Stepwise pyrolysis-gas chromatography is used to examine and characterize the carbonaceous matter in sedimentary rocks. Low-temperature steps remove material normally volatile or extracted by benzene-methanol. Successively-higher temperature steps degrade the insoluble carbonaceous matter (kerogen) into smaller molecular pieces. The sequential pyrolysis steps have the advantage of breaking the kerogen at several temperatures which may be related to bond type or strength. The pyrolysis product chromatograms from each step can be compared. The molecular sizes (chain length) of kerogens fragments can be determined. The results presented here show the molecules in the range C₁₁ to C₂₃ because: (1) they can be compared to normal petroleum source rock extractables; and (2) these large molecules give a feeling for the molecular construction of the kerogen.Green River and Antrim shales show low-temperature material which is indigenous and not modified compared to the pyrolyzed kerogen fragments in the range C₁₁C₂₃. Kupferletten shows low-temperature material of a narrow molecular weight range of C₁₅C₁₉ which is probably derived from the kerogen. Monterey shale low-temperature material appears to be unrelated to the kerogen as represented by its pyrolysis products. The Pierre shale kerogen shows molecules over the range C₁₁C₂₃. Kerogen from the Romney shale has no molecules large than C₈ in its pyrolysis products and no petroleum potential due to thermal and tectonic diagenesis.     

Normalizing XRF-scanner data: A cautionary note on the interpretation of high-resolution records from organic-rich lakes

X-ray fluorescence (XRF) scanning of unlithified, untreated sediment cores is becoming an increasingly common method used to obtain paleoproxy data from lake records. XRF-scanning is fast and delivers high-resolution records of relative variations in the elemental composition of the sediment. However, lake sediments display extreme variations in their organic matter content, which can vary from just a few percent to well over 50%. As XRF scanners are largely insensitive to organic material in the sediment, increasing levels of organic material effectively dilute those components that can be measured, such as the lithogenic material (the closed-sum effect). Consequently, in sediments with large variations in organic material, the measured variations in an element will to a large extent mirror the changes in organic material. It is therefore necessary to normalize the elements in the lithogenic component of the sediment against a conservative element to allow changes in the input of the elements to be addressed. In this study we show that Al, which is the lightest element that can be measured using the Itrax XRF-scanner, can be used to effectively normalize the elements of the lithogenic fraction of the sediment against variations in organic content. We also show that care must be taken when choosing resolution and exposure time to ensure optimal output from the measurements.     

Porous Structure Reconstruction Using Convolutional Neural Networks

The three-dimensional high-resolution imaging of rock samples is the basis for pore-scale characterization of reservoirs. Micro X-ray computed tomography (µ-CT) is considered the most direct means of obtaining the three-dimensional inner structure of porous media without deconstruction. The micrometer resolution of µ-CT, however, limits its application in the detection of small structures such as nanochannels, which are critical for fluid transportation. An effective strategy for solving this problem is applying numerical reconstruction methods to improve the resolution of the µ-CT images. In this paper, a convolutional neural network reconstruction method is introduced to reconstruct high-resolution porous structures based on low-resolution µ-CT images and high-resolution scanning electron microscope (SEM) images. The proposed method involves four steps. First, a three-dimensional low-resolution tomographic image of a rock sample is obtained by µ-CT scanning. Next, one or more sections in the rock sample are selected for scanning by SEM to obtain high-resolution two-dimensional images. The high-resolution segmented SEM images and their corresponding low-resolution µ-CT slices are then applied to train a convolutional neural network (CNN) model. Finally, the trained CNN model is used to reconstruct the entire low-resolution three-dimensional µ-CT image. Because the SEM images are segmented and have a higher resolution than the µ-CT image, this algorithm integrates the super-resolution and segmentation processes. The input data are low-resolution µ-CT images, and the output data are high-resolution segmented porous structures. The experimental results show that the proposed method can achieve state-of-the-art performance.     

Numerical study of mechanism of fold formation in a laminated rock

A set of large deformation experiments are presented to simulate folding pattern at various energy states during formation. In order to numerically simulate this phenomenon, a rectangular layer of shale is generated and compressed at various strain rates. The results reveal the variation in distribution of stress along the length of the bed. The stress distribution during elastic behaviour of shale bed at low compression rate and the change in stress distribution leading to rupture at high compression rates is discussed. Wavelength, limb length, bulk shortening, stress distribution, displacement of particles along the length of the bed is considered for comparative study of the fold pattern generated at various compression rates. The nature and position of crack generated during the formation of fold is also explained. After rupture in shale bed, the generation of fault and stress distribution in limbs of fold sliding over one another is also described.     

Numerical evaluation of mean-field homogenisation methods for predicting shale elastic response

Homogenisation techniques have been successfully used to estimate the mechanical response of synthetic composite materials, due to their ability to relate the macroscopic mechanical response to the material microstructure. The adoption of these mean-field techniques in geo-composites such as shales is attractive, partly because of the practical difficulties associated with the experimental characterisation of these highly heterogeneous materials. In this paper, numerical modelling has been undertaken to investigate the applicability of homogenisation methods in predicting the macroscopic, elastic response of clayey rocks. The rocks are considered as two-level composites consisting of a porous clay matrix at the first level and a matrix-inclusion morphology at the second level. The simulated microstructures ranged from a simple system of one inclusion/void embedded in a matrix to complex, random microstructures. The effectiveness and limitations of the different homogenisation schemes were demonstrated through a comparative evaluation of the macroscopic elastic response, illustrating the appropriate schemes for upscaling the microstructure of shales. Based on the numerical simulations and existing experimental observations, a randomly distributed pore system for the micro-structure of porous clay matrix has been proposed which can be used for the subsequent development and validation of shale constitutive models. Finally, the homogenisation techniques were used to predict the experimental measurements of elastic response of shale core samples. The developed methodology is proved to be a valuable tool for verifying the accuracy and performance of the homogenisation techniques.