Characteristics and discovery significance of the Upper Triassic–Lower Jurassic marine shale oil in Qiangtang Basin,China

Mesozoic marine shale oil was found in the Qiangtang Basin by a large number of hydrocarbon geological surveys and shallow drilling sampling.Based on systematic observation and experimental analysis of outcrop and core samples,the deposition and development conditions and characteristics of marine shale are revealed,the geochemical and reservoir characteristics of marine shale are evaluated,and the layers of marine shale oil in the Mesozoic are determined.The following geological understandings are obtained.First,there are two sets of marine organic-rich shales,the Lower Jurassic Quse Formation and the Upper Triassic Bagong Formation,in the Qiangtang Basin.They are mainly composed of laminated shale with massive mudstone.The laminated organic-rich shale of the Quse Formation is located in the lower part of the stratum,with a thickness of 50–75 m,and mainly distributed in southern Qiangtang Basin and the central-west of northern Qiangtang Basin.The laminated organic-rich shale of the Bagong Formation is located in the middle of the stratum,with a thickness of 250–350 m,and distributed in both northern and southern Qiangtang Basin.Second,the two sets of laminated organic-rich shales develop foliation,and various types of micropores and microfractures.The average content of brittle minerals is 70%,implying a high fracturability.The average porosity is 5.89%,indicating good reservoir physical properties to the level of moderate–good shale oil reservoirs.Third,the organic-rich shale of the Quse Formation contains organic matters of types II1 and II2,with the average TOC of 8.34%,the average content of chloroform bitumen'A'of 0.66%,the average residual hydrocarbon generation potential(S1+S2)of 29.93 mg/g,and the Ro value of 0.9%–1.3%,meeting the standard of high-quality source rock.The organic-rich shale of the Bagong Formation contains mixed organic matters,with the TOC of 0.65%–3.10%and the Ro value of 1.17%–1.59%,meeting the standard of moderate source rock.Fourth,four shallow wells(depth of 50–250 m)with oil shows have been found in the organic shales at 50–90 m in the lower part of the Bagong Formation and 30–75 m in the middle part of the Quse Formation.The crude oil contains a high content of saturated hydrocarbon.Analysis and testing of outcrop and shallow well samples confirm the presence of marine shale oil in the Bagong Formation and the Quse Formation.Good shale oil intervals in the Bagong Formation are observed in layers 18–20 in the lower part of the section,where the shales with(S0+S1)higher than 1 mg/g are 206.7 m thick,with the maximum and average(S0+S1)of 1.92 mg/g and 1.81 mg/g,respectively.Good shale oil intervals in the Quse Formation are found in layers 4–8 in the lower part of the section,where the shales with(S0+S1)higher than 1 mg/g are 58.8 m thick,with the maximum and average(S0+S1)of 6.46 mg/g and 2.23 mg/g,respectively.

Controlling Factors of Organic Nanopore Development: A Case Study on Marine Shale in the Middle and Upper Yangtze Region, South China

The Upper Ordovician Wufeng-Lower Silurian Longmaxi and the Lower Cambrian Qiongzhusi shales are the major targets for shale gas exploration and development in China.Although the two organic-rich shales share similar distribution ranges and thicknesses,they exhibit substantially different exploration and development results.This work analyzed the nanopore structures of the shale reservoirs in this region.Pore development of 51 shale samples collected from various formations and locations was compared using the petromineralogical,geochemical,structural geological and reservoir geological methods.The results indicate that the reservoir space in these shales is dominated by organic pores and the total pore volume of micropores,mesopores,macropores in different tectonic areas and formations show different trends with the increase of TOC.It is suggested that organic pores of shale can be well preserved in areas with simple structure and suitable preservation conditions,and the shale with smaller maximum ancient burial depth and later hydrocarbongeneration-end-time is also more conducive to pore preservation.Organic pore evolution models are established,and they are as follows:①Organic matter pore development stage,②Early stage of organic matter pore destruction,and③late stage of organic matter pore destruction.The areas conducive to pore development are favorable for shale gas development.Research results can effectively guide the optimization and evaluation of favorable areas of shale gas.

Characterization of natural fractures in deep-marine shales: a case study of the Wufeng and Longmaxi shale in the Luzhou Block Sichuan Basin, China

Natural fractures are of crucial importance for oil and gas reservoirs,especially for those with ultralow permeability and porosity.The deep-marine shale gas reservoirs of the Wufeng and Longmaxi Formations are typical targets for the study of natural fracture characteristics.Detailed descriptions of full-diameter shale drill core,together with 3D Computed Tomography scans and Formation MicroScanner Image data acquisition,were carried out to characterize microfracture morphology in order to obtain the key parameters of natural fractures in such system.The fracture type,orientation,and their macroscopic and microscopic distribution features are evaluated.The results show that the natural fracture density appears to remarkably decrease in the Wufeng and Longmaxi Formations with increasing the burial depth.Similar trends have been observed for fracture length and aperture.Moreover,the natural fracture density diminishes as the formation thickness increases.There are three main types of natural fractures,which we interpret as(I)mineral-filled fractures(by pyrite and calcite),i.e.,veins,(II)those induced by tectonic stress,and(III)those formed by other processes(including diagenetic shrinkage and fluid overpressure).Natural fracture orientations estimated from the studied natural fractures in the Luzhou block are not consistent with the present-day stress field.The difference in tortuosity between horizontally and vertically oriented fractures reveals their morphological complexity.In addition,natural fracture density,host rock formation thickness,average total organic carbon and effective porosity are found to be important factors for evaluating shale gas reservoirs.The study also reveals that the high density of natural fractures is decisive to evaluate the shale gas potential.The results may have significant implications for evaluating favorable exploration areas of shale gas reservoirs and can be applied to optimize hydraulic fracturing for permeability enhancement.

Geological conditions and reservoir characteristics of various shales in major shalehosted regions of China

China is home to shales of three facies:Marine shale,continental shale,and marine-continental transitional shale.Different types of shale gas are associated with significantly different formation conditions and major controlling factors.This study compared the geological characteristics of various shales and analyzed the influences of different parameters on the formation and accumulation of shale gas.In general,shales in China’s several regions exhibit high total organic carbon(TOC)contents,which lays a sound material basis for shale gas generation.Marine strata generally show high degrees of thermal evolution.In contrast,continental shales manifest low degrees of thermal evolution,necessitating focusing on areas with relatively high degrees of thermal evolution in the process of shale gas surveys for these shales.The shales of the Wufeng and Silurian formations constitute the most favorable shale gas reservoirs since they exhibit the highest porosity among the three types of shales.These shales are followed by those in the Niutitang and Longtan formations.In contrast,the shales of the Doushantuo,Yanchang,and Qingshankou formations manifest low porosities.Furthermore,the shales of the Wufeng and Longmaxi formations exhibit high brittle mineral contents.Despite a low siliceous mineral content,the shales of the Doushantuo Formation feature a high carbonate mineral content,which can increase the shales’brittleness to some extent.For marine-continental transitional shales,where thin interbeds of tight sandstone with unequal thicknesses are generally found,it is recommended that fracturing combined with drainage of multiple sets of lithologic strata should be employed to enhance their shale gas production.

Thermal maturation as revealed by micro-Raman spectroscopy of mineral-organic aggregation (MOA) in marine shales with high and over maturities

Laser Raman spectroscopy of organic matter in coals and sedimentary rocks has been increasingly investigated to assess thermal maturity.Pure organic matter such as vitrinite and solid bitumen,as well as isolated kerogen are definitely selected for this purpose,but there has been no systematic report on the Raman spectral parameters directly based on mineral-organic aggregations(MOA)in shales.In this paper,the Raman spectral characteristics and parameters of MOA in two sets of marine shale samples from southern China with either different TOC contents(TOC=0.10–4.59%)or different maturities(BRo=1.71–4.57%)were investigated.It was found that the Raman technique is very sensitive to the organic matter in MOA.As the TOC content of the shales reaches about 0.60%,perfect Raman spectra with D and G bands derived from organic matter in MOAwere obtained,and the Raman parameters of MOA are in good agreement with those of its associated solid bitumen,and can indicate the thermal maturity just like those of solid bitumen.Using the Raman parameters of MOA is a potential alternative way to estimate maturity levels of high and over mature shales,especially those lower Paleozoic and Precambrian shales that lack macerals suitable for reflectance or Raman measurements.

Pore Structure and Multi-Scale Fractal Characteristics of Adsorbed Pores in Marine Shale:A Case Study of the Lower Silurian Longmaxi Shale in the Sichuan Basin,China

Exploration practice indicates that free gas is the key to the large-scale development of shale gas,while adsorbed gas is also of great significance to the sustainable development of shale gas,and thus systematic researches on absorbed pores are needed.To date,researches on pore structure and multi-scale fractal characteristics of absorbed pores in marine shale are obviously insufficient,limited the understanding of gas production behavior from shale reservoir.In this study,total organic carbon(TOC),X-ray diffraction(XRD),CH_(4) adsorption,field emission electron microscopy(FE-SEM),and low temperature gas(i.e.,CO_(2)and N_(2))adsorption/desorption analyses were conducted on 10 continuously core samples from the Lower Silurian Longmaxi shale in the Fuling region of Sichuan Basin,China.The results indicate that the TOC content of marine shale samples changes from 0.95%to 4.55%with an average of 2.62%,showing an increasing trend with the increase of burial depth;moreover,quartz and clay are the dominated mineral compositions in marine shale,and they show a certain negative correlation.FE-SEM analysis indicates that almost all pore types in marine shale are related to organic matter(OM).Hysteresis loops of marine shale samples mainly belong to Type H2,further indicating that the pores in marine shale are mainly ink-bottle pores(i.e.,OM pores);moreover,adsorption isotherms obtained from CO_(2)adsorption data all belong to typeⅠ,indicating microporous properties for all shale samples.Comprehensive analysis indicates that pore volume and pore surface area of adsorbed pores(<300 nm)is mainly provided by the pores within the pore range of 0.6–0.7,0.80–0.85,and 1.7–5.0 nm.Based on the micropore filling model and the Frenkel-Halsey-Hill(FHH)model,multiscale fractal dimensions(D1,D2,and D3)are calculated from gas adsorption data(i.e.,CO_(2)and N_(2)),corresponding to part of micropore(0.6–1.1 nm),small-mesopore(1.7–5.0 nm),big-mespore and part of macropore(5.0–300 nm),respectively.Relationships between shale compositions,pore structure,and fractal dimensions(D1,D2,and D3)indicate that pore structure and multi-scale fractal characteristics of absorbed pores in marine shale are obviously influenced by the contents of TOC and quartz,while clay minerals have little effect on them.Comprehensive analysis indicates that the complexity of marine shale pores within the range of 0.6–1.1 and 1.7–5.0 nm has significant effects on CH_(4) adsorbability,while the larger pores(5.0–300 nm)almost have no effect.

Determination of gas adsorption capacity in organic-rich marine shale: a case study of Wufeng-Lower Longmaxi Shale in the southeast Sichuan Basin

Determination of gas adsorption capacity under geological conditions is essential in evaluating shale gas resource potential.A quantitative determination of gas adsorption capacity was proposed through 1)investigating controlling geological factors(including both internal ones and external ones)of gas adsorption capacity in organic-rich marine shale with geochemical analysis,XRD diffraction,field-emission scanning electron microscopy,and methane sorption isotherms;2)defining the relationship between gas adsorption capacity and single controlling factor;3)establishing a comprehensive determination model with the consideration of all these controlling factors.The primary controlling factors of the sorption capacity for the studied O3wLower S1l shale are TOC,illite and quartz,temperature,pressure,Ro,and moisture(water saturation).Specifically,TOC,thermal maturity,illite,and pressure are positively correlated with sorption capacity,whereas,quartz and temperature contribute negatively to the sorption capacity.We present the quantitative model along with application examples from the Wufeng-Lower Longmaxi Shale in the southeast Sichuan Basin,west China,to demonstrate the approach in shale gas evaluation.The result shows that the comprehensive determination model provides a good and unbiased estimate of gas adsorption capacities with a high correlation coefficient(0.96)and bell-shaped residues centered at zero.

Influence of structural damage on evaluation of microscopic pore structure in marine continental transitional shale of the Southern North China Basin:A method based on the low-temperature N2 adsorption experiment

Structural damage from sample preparation processes such as cutting and polishing may change the pore structure of rocks.However,changes in pore structure caused by this structural damage from crushing and its effect on marine continental transitional shale have not been well documented.The changes of microscopic pore structure in marine continental transitional shale during the sample preparation have important research value for subsequent exploration and development of shale gas.In this study,the pore structures of transitional shale samples from the Shanxi-Taiyuan Formation of the Southern North China Basin under different degrees of damage were analyzed through low-temperature N;adsorption experiments,combined with X-ray diffraction,total organic carbon,vitrinite reflectance analysis,and scanning electron microscopy.The results showed that(1)With increasing structural damage,the specific surface area(SSA)changed within relatively tight bounds,while the pore volume(PV)varied significantly,and the growth rate(maximum)exhibited a certain critical value with the crushing mesh number increasing from 20 to 200.(2)The ratio of SSA to PV can be used as a potential proxy for evaluating the influence of changes in the pore structure.(3)Correlation analysis revealed that the microscopic pore structure of marine continental transitional shale from the Shanxi-Taiyuan Formations is mainly controlled by organic matter and clay minerals.Clay minerals play a leading role in the development of microscopic pores and changes in pore structure.

Fracability Evaluation of Shale of the Wufeng-Longmaxi Formation in the Changning Area, Sichuan Basin

The fracturing technology for shale gas reservoir is the key to the development of shale gas industrialization.It makes much sense to study the mechanical properties and deformation characteristics of shale,due to its close relationship with the fracability of shale gas reservoir.This paper took marine shale in the Changning area,southern Sichuan Basin of China as the research object.Based on field profile and hand specimen observation,we analyzed the development of natural fractures and collected samples from Wufeng Formation and Longmaxi Formation.Combining with the indoor experiment,we investigated the macroscopic and microscopic structural features and the remarkable heterogeneity of shale samples.Then we illustrated the mechanics and deformation characteristics of shale,through uniaxial compression test and direct shear test.The shale has two types of fracture modes,which depend on the angular relation between loading direction and the bedding plane.Besides,the Wufeng shale has a higher value of brittleness index than the Longmaxi shale,which was calculated using two methods,mechanical parameters and mineral composition.Given the above results,we proposed a fracability evaluation model for shale gas reservoir using the analytic hierarchy process.Four influence factors,brittleness index,fracture toughness,natural fractures and cohesive force,are considered.Finally,under the control of normalized value and weight coefficient of each influence factor,the calculations results indicate that the fracability index of the Wufeng Formation is higher than that of the Longmaxi Formation in Changning area,southern Sichuan Basin.

“Extreme utilization”development of deep shale gas in southern Sichuan Basin,SW China

To efficiently develop deep shale gas in southern Sichuan Basin,under the guidance of“extreme utilization”theory,a basic idea and solutions for deep shale gas development are put forward and applied in practice.In view of multiple influencing factors of shale gas development,low single-well production and marginal profit of wells in this region,the basic idea is to establish“transparent geological body”of the block in concern,evaluate the factors affecting shale gas development through integrated geological-engineering research and optimize the shale gas development of wells in their whole life cycle to balance the relationship between production objectives and development costs.The solutions are as follows:(1)calculate the gold target index and pinpoint the location of horizontal well drilling target,and shale reservoirs are depicted accurately by geophysical and other means to build underground transparent geological body;(2)optimize the drilling and completion process,improve the adaptability of key tools by cooling,reducing density and optimizing the performance of drilling fluid,the“man-made gas reservoir”is built by comprehensively considering the characteristics of in-situ stress and fractures after the development well is drilled;(3)through efficient management,establishment of learning curve and optimization of drainage and production regime,the development quality and efficiency of the well are improved across its whole life cycle,to fulfil“extreme utilization”development of shale gas.The practice shows that the estimated ultimate recovery of single wells in southern Sichuan Basin increase by 10%-20%than last year.

Geological Characteristics of Shale Gas in Different Strata of Marine Facies in South China

In the Middle and Upper Yangtze region of South China,there are well developed sets of marine shale strata.Currently only Wufeng Longmaxi shale gas has been developed in scale,while the Sinian and Cambrian shale gas are still under exploration.The various shale strata show different characteristics in lithological features,such as lithofacies types and reservoir physical properties,which are due to the influence of tectonic pattern,sedimentary environment,and diagenesis caused by tectonic subsidence.This will affect the later fracturing technology and fracturing effect.The shale reservoirs of Sinian doushantuo,Cambrian Niutitang,Upper Ordovician Wufeng,and the Lower Silurian Longmaxi Formation shale were evaluated and compared with each other with respect to their sedimentary environments,lithofacies,minerals compositions,and micro pore characteristics.The reservoir characteristics of the shale and the main control factors of shale gas enrichment were summarized in this study.

Experimental study of water imbibition characteristics of the lacustrine shale in Sichuan Basin

Through the stimulation method of large-scale hydraulic fracturing,the spontaneous imbibition capacity of the water phase in the shale reservoir has great influence on the effect of stimulation.Generally,the lacustrine shale has the characteristics of high clay minerals content,strong expansibility,development of nanopores and micro-pores,and underdevelopment of fractures,which leads to the unclear behavior of spontaneous imbibition of aqueous phase.The lacustrine shale of Da'anzhai Member and marine shale of Longmaxi Formation in Sichuan Basin were selected to prepare both the shale matrix sample and fractured shale sample,and the spontaneous imbibition experiment of simulated formation water was carried out.By means of an XRD test,SEM observation,nuclear magnetic resonance test and linear expansion rate test,the mineral composition,the structure of pores and fractures,the capacity of hydration and expansion of both lacustrine and marine shale are compared and analyzed.The results show that the average spontaneous imbibition rate of lacustrine shale is 60.8%higher than that of marine shale within the initial 12 hours of imbibition.The lacustrine shale has faster imbibition rate than the marine shale in the initial stage of spontaneous imbibition.However,the lacustrine shale has underdeveloped pores and fractures,as well as poor connectivity of pores.Besides,the strong hydration and expansion of clay minerals can easily lead to dispersion and migration of clay minerals on the fracture surface,which will plug up the seepage channels,resulting in poor capacity of spontaneous imbibition.The spontaneous imbibition rate in the middle and late stage of Lacustrine shale is obviously lower than that of the marine shale.The overall spontaneous imbibition rate ability of the lacustrine shale is less than that of the marine shale.According to the characteristics of water imbibition of lacustrine shale,considering the dual effects of hydration expansion of clay minerals on the effective reconstructed volume,the microfractures can be initiated and extended by fully utilizing the hydration of shale.Acidification treatment,oxidation treatment or high temperature treatment can be used to expand pore space,enhance water phase imbibition capacity and improve multi-scale mass transfer capacity of the lacustrine shale.

Micron-to nano-pore characteristics in the shale of Longmaxi Formation,southeast Sichuan Basin

For shale of Lower Silurian Longmaxi Formation in Chongqing,southeast Sichuan Basin,characteristics of micro-nano pores in marine shale reservoirs were well studies by means of Field-Emission Scanning Electron Microscope and Low-temperature Low-pressure Adsorption Experiment of CO_(2)and N_(2).Results showed that six types of pore were developed in the shale of Longmaxi Formation,i.e.,organic pores,intergranular pores,intragranular pores,intercrystalline pores,dissolution pores and microfractures,among which the organic pores and intragranular pores in interlayers of clay minerals were most developed,and a plenty of dissolution pores were also well developed because of high thermal evolution degree.BET specific surface area of the shale in Longmaxi Formation ranged from 3.5 to 18.1 m^(2)/g,BJH total pore volume was from 0.00234 to 0.01338 cm^(3)/g,DA specific surface area of micropores vaired from 1.3 to 7.3 m^(2)/g,and DA pore volume ranged from 0.00052 to 0.00273 cm^(3)/g.The specific surface area of micropores in the shale accounted for 23.1%-80.2%of total specific surface area with an average of 50.3%,and the pore volume of micropores accounted for 12.1%-48.5%of total pore volume with an average of 32.3%.Micropore was the main storage space in shale reservoir for methane adsorption,that because capacities of specific surface area provided by micropores were considerably greater than those provided by mesopores and macropores.Pore size distribution of the shale was complex,and multiple different peaks occurred in the pore size curves,showing two or three peaks in the range from 0 to 100 nm and four peaks occasionally.TOC had a good linear relationship with pore structure parameters of micropores,mesopores t macropores and total pores in the shale,indicating that TOC was the most important control factor for micron-to nano-pore structure in the shale.After normalization of pore structure parameters to TOC,the pore structure parameters of total pores and mesopores t macropores,had positive linear relationships with content of clay minerals but negative linear relationships with content of brittle minerals,indicating that clay minerals and brittle minerals mainly controlled development of mesopores and macropores in the shale.

Maturity Assessment of the Lower Cambrian and Sinian Shales Using Multiple Technical Approaches

The Lower Cambrian Niutitang and Sinian Doushantuo shales are the most important and widespread source rocks and target layers in South China. Reliable data of the thermal maturity of organic matter(OM) is widely used to assess hydrocarbon generation and is a key property used in determining the viability and hydrocarbon potential of these new shales. Nevertheless, traditional thermal maturity indicators are no longer suited to the vitrinite-lack marine shales. This study aims to combine high throughput Raman and infrared spectroscopy analysis to confirm and validate the thermal maturity in comparison with the bitumen reflectance(R_(b)). Raman parameters such as the differences between the positions of the two bands(V_(G)–V_(D)) are strong parameters for calculating the thermal maturity in a large vitrinite reflectance(R_(o)) ranging from 1.60% to 3.80%. The infrared spectroscopy analysis indicates that the aromatic C=C bands and CH_(2)/CH_(3) aliphatic groups both are closely correlated with thermal maturity. The calculated R_(o) results from Raman and infrared spectroscopy are in strong coincidence with the R_(b). The relationships between R_(b) and pore volumes/surface areas(calculated from N_(2) adsorption) indicate that the sample with R_(b) of 3.40% has the lowest pore volumes and surface areas. Focused ion beam scanning electron microscopy(FIB-SEM) observations of OM pores indicate that R_(o) of approximately 3.60% may be an upper limit for OM porosity development. Obviously, kerogen Raman and infrared spectroscopy can indicate methods for reducing the risk in assessing maturity with practical, low-cost accurate results. Exploration of shale gas in the high maturity(>3.40%–3.60%) region carries huge risks.