CN104237284A - Nuclear magnetic resonance detection method for brittle and hard shale microcrack damage - Google Patents
Nuclear magnetic resonance detection method for brittle and hard shale microcrack damage Download PDFInfo
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- CN104237284A CN104237284A CN201410553942.2A CN201410553942A CN104237284A CN 104237284 A CN104237284 A CN 104237284A CN 201410553942 A CN201410553942 A CN 201410553942A CN 104237284 A CN104237284 A CN 104237284A
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Abstract
The invention provides a nuclear magnetic resonance detection method for brittle and hard shale microcrack damage. The nuclear magnetic resonance detection method comprises the steps of firstly, processing a test sample, soaking the test sampling in distilled water, taking out the test sample in different soaking time, and then performing nuclear magnetic resonance detection on the test sample and obtaining a spin echo train deamplification signal, which is a superposed signal of water signals in pores different in size, by performing CPMG pulse sequence testing on the test sample, secondly, inverting the spin echo train signal to obtain the distribution diagram, the spectrum area value and the scale value of each peak of a T2 spectrum, and finally, performing nuclear magnetic resonance imaging measurement and analysis and reflecting the microstructure distribution characteristics inside the test sample by use of a nuclear magnetic resonance image; the size distribution condition of the internal pores of the test sample can be visually shown and the dynamic damage evolution process of the internal structure of the test sample under hydration is displayed; the nuclear magnetic resonance detection method for brittle and hard shale microcrack damage is used for analyzing the dynamic development condition of the cracks of the hydrated brittle and hard shale by virtue of nuclear magnetic resonance and has practical guidance significance for guiding field plugging and leaking stoppage.
Description
Technical field
The present invention relates to well-bore stability technology field, particularly relate to the magnetic resonance detection method of crisp rigid mud shale microfracture damage.
Background technology
Borehole well instability problem is the challenge that in Process of Oil Well Drilling, ubiquity also perplexs petroleum industrial circle always.Wherein mud shale unstability just accounts for more than 90%, and therefore some researcher thinks that Wellbore Stability is exactly shale stability problem.In crisp rigid mud shale, microfracture is grown on the one hand is the major reason causing borehole well instability, and higher drilling liquid pressure can be compressed into crack drilling fluid thus accelerate Shale Hydration, is unfavorable for wellbore stability; Hard brittle shale and entry well fluid interact on the other hand, a series of microphysics chemical change will be produced therein, change rock substance inner structure and mechanical property, make rock interior crack extesion, physical chemistry and mechanics effect two kinds of effects intercouple, and then affect the stability on stratum.In order to observe with the damage development of study of rocks inner structure until the process of breaking completely, Chinese scholars is studied by various rock fine observation mechanical test.Shi Bingzhong adopts CT imaging technique, and microcosmic discloses the rule of development in crack in hard brittle shale hydration process.
Nuclear magnetic resonance technique (NMR) as the novel detection mode of study of rocks microscopical structure, have harmless, repeatedly with the advantage such as quick.Current nuclear magnetic resonance technique, in petroleum engineering field, mainly through the research to aspects such as rock pore structure, reservoir rock pore fluid characteristics, carries out the application of evaluating reservoir and well logging well logging aspect.Yet there are no the research being applied to analyze shale hydration damage mechanisms.Nuclear magnetic resonance technique is utilized to carry out the test of T2 and NMR imaging to the sample of different soak time, by analyzing T2 T
2spectral structure, T
2the change of area under spectrum and NMR imaging, analyze underbead crack damage development process after shale hydration.Concrete directive significance is had to on-the-spot shutoff borehole wall crack.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide the magnetic resonance detection method of crisp rigid mud shale microfracture damage, having real directive significance to guide field shutoff, leak stopping.
In order to achieve the above object, the technical scheme that the present invention takes is:
The magnetic resonance detection method of crisp rigid mud shale microfracture damage, comprises the following steps:
The first step, is processed into sample the right cylinder that diameter is 25 millimeters, length is 50 millimeters by industry standard;
Second step, is immersed in sample in distilled water, takes out sample after soaking 10min;
3rd step, carrying out magnetic resonance detection to the sample through soaking, by carrying out the test of CPMG pulse train to sample, obtaining the deamplification of spin echo string, and signal is the superposition of water signal in different large fine porosity; Utilize NMR (Nuclear Magnetic Resonance) relaxation time reversal fitting software to carry out inverting to spin echo string signal, obtain T
2the distribution plan composed, area under spectrum value and each peak proportion value;
4th step, utilizes MiniMR MRI software to measure sample, is reflected the micromechanism distribution characteristics of sample inside by nuclear magnetic resonance image;
5th step, continues to soak to complete sample, takes out respectively, carry out nuclear-magnetism experiment when 30min, 1h, 2h, 4h, 6h, 8h, 1d, 3d, 5d, repeat the 3rd step and the 4th step;
6th step, obtains the T of same sample under different soak time by the 5th step
2analyze under spectrum is put into a coordinate system, according to nuclear magnetic resonance principle, T
2relaxation is determined by surface relaxation, and Surface Relaxation is relevant with media surface area, and Media Ratio surface the ratio of volume of voids V (the porous medium pore surface area S with) is larger, then relaxation is stronger, and vice versa, T
2surface is expressed as:
ρ in formula
2for T
2surface Relaxation intensity; (S/V)
holefor pore surface area and the ratio of volume of voids, then obtain T
2with the pass of aperture r be:
Fs is called geometrical form factors, and relevant with pore space size by the relaxation time of above formula visible hole inner fluid, hole is less, and specific area is larger, and the impact of surface interaction is stronger, T
2time is also shorter, relaxation time T
2be one to one with average pore size r, utilize T
2pore size and pore diameter distribution thereof are evaluated in distribution;
7th step, to the T that the 5th step inverting obtains
2area under spectrum is analyzed, nuclear magnetic resonance T2 T
2the integral area of spectrum to be proportional in sample contained fluid number, it is equal to or slightly less than the net porosity of sample, and the hole quantity in corresponding aperture is relevant with the size of peak area, after analyzing same sample difference soak time, T
2the change of area under spectrum and each peak proportion, obtain the change of cicada sample aperture gap volume, quantity;
8th step, the Magnetic resonance imaging result of the different soak time of same sample that the 5th step obtains is analyzed, intercept the cross section axially vertical with sample and carry out imaging, in image, black is background color, the region of turning white is hydrone region, what represent is aperture ranges, the brightness of image reflects the number of sample containing water amount, white speck is more, mean that sample hole is larger, otherwise, then hole is less, intuitively can find out the pore size distribution situation of sample inside like this, illustrate sample under hydration, the damage evolution process of inner structure.
Beneficial effect of the present invention: the present invention by nuclear magnetic resonance technique means, analyzes the active development situation in crack after crisp rigid shale hydration, has the directive significance of reality to guide field shutoff, leak stopping.
Accompanying drawing explanation
Fig. 1 is the T that the sample of embodiment soaks in 1h
2spectrum variation diagram.
Fig. 2 is the T that the sample of embodiment soaks in 1d
2spectrum variation diagram.
Fig. 3 is that the T2 that the sample of embodiment soaks in 5d composes variation diagram.
Crackle is there is in Fig. 4 after the sample of embodiment soaks.
Fig. 5 is the NMR imaging figure of the sample immersion 1h of embodiment.
Fig. 6 is the NMR imaging figure of the sample immersion 8h of embodiment.
Fig. 7 is the NMR imaging figure of the sample immersion 1d of embodiment.
Fig. 8 is the NMR imaging figure of the sample immersion 3d of embodiment.
Fig. 9 is the NMR imaging figure of the sample immersion 5d of embodiment.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in detail.
The magnetic resonance detection method of crisp rigid mud shale microfracture damage, comprises the following steps:
The first step, is processed into sample the right cylinder that diameter is 25 millimeters, length is 50 millimeters by industry standard;
Second step, is immersed in sample in distilled water, takes out sample after soaking 10min;
3rd step, carrying out magnetic resonance detection to the sample through soaking, by carrying out the test of CPMG pulse train to sample, obtaining the deamplification of spin echo string, and signal is the superposition of water signal in different large fine porosity; Utilize NMR (Nuclear Magnetic Resonance) relaxation time reversal fitting software to carry out inverting to spin echo string signal, obtain T
2the distribution plan composed, area under spectrum value and each peak proportion value;
4th step, utilizes MiniMR MRI software to measure sample, is reflected the micromechanism distribution characteristics of sample inside by nuclear magnetic resonance image;
5th step, continues to soak to complete sample, takes out respectively, carry out nuclear-magnetism experiment when 30min, 1h, 2h, 4h, 6h, 8h, 1d, 3d, 5d, repeat the 3rd step and the 4th step;
6th step, obtains the T of same sample under different soak time by the 5th step
2analyze under spectrum is put into a coordinate system, according to nuclear magnetic resonance principle, the T of sample
2relaxation is determined by surface relaxation, and Surface Relaxation is relevant with media surface area, and Media Ratio surface the ratio of volume of voids V (the porous medium pore surface area S with) is larger, then relaxation is stronger, and vice versa, T
2surface is expressed as:
ρ in formula
2for T
2surface Relaxation intensity; (S/V)
holefor pore surface area and the ratio of volume of voids, then obtain T
2with the pass of aperture r be:
Fs is called geometrical form factors, and relevant with pore space size by the relaxation time of above formula visible hole inner fluid, hole is less, and specific area is larger, and the impact of surface interaction is stronger, T
2time is also shorter, relaxation time T
2be one to one with average pore size r, utilize T
2pore size and pore diameter distribution thereof are evaluated in distribution,
With reference to Fig. 1, in initial 1h, the T of sample
2spectral structure main manifestations is 2 peaks, and the 1st peak-to-peak signal is strong, and the 2nd peak-to-peak signal is more weak, illustrates that the first peak representing fine porosity is in the great majority, and along with the prolongation of soak time, the changes in amplitude at first peak is not obvious; Second peak of the slightly large scale microporosity that right side is corresponding, change obviously, there occurs and moves to right, namely to macroporous T
2direction offsets, and shows to be introduced in inner microfracture in water rate, occurs obvious Crack Extension, cause macropore T
2the NMR signal intensity of spectrum increases,
With reference to Fig. 2, after the immersion of 8h, T
2on spectrogram, the amplitude at first peak of corresponding small size microporosity obviously increases, the new hole constantly producing and expand, and make pore-size and volume constantly become large, therefore NMR signal intensity increases.Along with the prolongation of soak time, part T
2spectrum is 3 peak figure, the 2nd peak of the large scale microfissure of right side correspondence, continues to move to the right, illustrates that microfracture is constantly expanded under hydration, bifurcated, defines more microfracture, shows that more serious aquation damage has appearred in sample,
With reference to Fig. 3, after the immersion of 1d, T
2the small size microporosity that first peak on distribution plan is corresponding, the amplitude of variation at peak increases further, illustrate that new microporosity is also constantly producing and expansion, 2nd, 3 the large scale crack corresponding to peak on right side, at this moment change is little, the even synthesis had peak, illustrates that oversized hole crazing line has completed the process of microcrack initiation-expansion-bifurcated-merger-through-macroscopic failure; With reference to Fig. 4, Figure 4 shows that sample soaks the situation of 5 days, can find out: macroscopical visible crackle has appearred in specimen surface;
7th step, to the T that the 5th step inverting obtains
2area under spectrum is analyzed, nuclear magnetic resonance T2 T
2the integral area of spectrum to be proportional in sample contained fluid number, it is equal to or slightly less than the net porosity of sample, and the hole quantity in corresponding aperture is relevant with the size of peak area, after analyzing same sample difference soak time, T
2the change of area under spectrum and each peak proportion, obtain the change of cicada sample aperture gap volume, quantity;
Subordinate list is sample nuclear magnetic resonance area under spectrum under different soak time
T can be found out from subordinate list
2area under spectrum increases gradually, show the prolongation along with soak time, sample volume of voids increases, and first peak of corresponding small size microporosity accounts for about 90% of the total area, show that undersized microporosity accounts for the overwhelming majority, after 1h soaks, the change of first peak proportion is little, and the second peak changes greatly relatively, show that the inner large scale hole of sample increases very fast, namely there is the expansion of obvious micro-cracks damage in sample inside, soak time more than after 8h, T
2there is again obvious change in area under spectrum, and has occurred the 3rd peak, illustrates simultaneously and the expansion of adjoint micro-crack, bring out again and create some new bifurcated micro-cracks, crack number now in sample is more and long, causes sample internal injury to strengthen, T after 1d
2the continuation of area under spectrum becomes large, first peak accounting example of corresponding small size microporosity also obviously increases, but corresponding large scale hole second peak accounting example diminishes, 3rd peak even disappears, illustrate that microporosity is also constantly producing and expansion, the merger of oversized hole crazing line penetrates into macroscopic failure, and illustrate that the aquation damage of sample changes greatly early stage, later stage change slowly;
8th step, the Magnetic resonance imaging result of the different soak time of same sample that the 5th step obtains is analyzed, intercept the cross section axially vertical with sample and carry out imaging, in image, black is background color, the region of turning white is hydrone region, what represent is aperture ranges, the brightness of image reflects the number of sample containing water amount, white speck is more, means that sample hole is larger, otherwise, then hole is less, intuitively can find out the pore size distribution situation of sample inside like this, illustrate sample under hydration, the damage evolution process of inner structure.
Be soak the sample Magnetic resonance imaging figure of 1h with reference to Fig. 5, Fig. 5, in figure, white bright spot is uneven and few, and cross section hole quantity is few, and based on small size hole, moisturely in hole mostly is irreducible water.The subregional dark images in figure middle part, shows that the sample structure in this region is fine and close, mays be seen indistinctly one and runs through the macroporous structure (microfracture) in cross section, illustrates that sample unevenness obviously, containing initial micro-cracks damage at cross-sectional right side.
With reference to the sample Magnetic resonance imaging image that Fig. 6, Fig. 6 are after the immersion of 8h, brightness of image obviously increases, and original macroporous structure (micro-crack) brightness increases, and the shape size in crack mays be seen indistinctly.
With reference to Fig. 7, Fig. 7 is the sample Magnetic resonance imaging image after the immersion of 1 day, and brightness of image grow, obviously can find out the size and shape in hole crack, and crack extends along the radial direction of sample, illustrates that aquation makes specimen cross section hole quantity and size all improve to some extent.
Be respectively the sample Magnetic resonance imaging image after 3 days and 5 days are soaked with reference to Fig. 8 and Fig. 9, Fig. 8 and Fig. 9, two pictures have similar pore structural information.The bright dark inequality of image, distribution of pores is very uneven, has all occurred larger hole at the inside of sample, periphery, and porosity communication.
Claims (1)
1. the magnetic resonance detection method of crisp rigid mud shale microfracture damage, is characterized in that, comprise the following steps:
The first step, is processed into sample the right cylinder that diameter is 25 millimeters, length is 50 millimeters by industry standard;
Second step, is immersed in sample in distilled water, takes out sample after soaking 10min;
3rd step, carrying out magnetic resonance detection to the sample through soaking, by carrying out the test of CPMG pulse train to sample, obtaining the deamplification of spin echo string, and signal is the superposition of water signal in different large fine porosity; Utilize NMR (Nuclear Magnetic Resonance) relaxation time reversal fitting software to carry out inverting to spin echo string signal, obtain T
2the distribution plan composed, area under spectrum value and each peak proportion value;
4th step, utilizes MiniMR MRI software to measure sample, is reflected the micromechanism distribution characteristics of sample inside by nuclear magnetic resonance image;
5th step, continues to soak to complete sample, takes out respectively, carry out nuclear-magnetism experiment when 30min, 1h, 2h, 4h, 6h, 8h, 1d, 3d, 5d, repeat the 3rd step and the 4th step;
6th step, obtains the T of same sample under different soak time by the 5th step
2analyze under spectrum is put into a coordinate system, according to nuclear magnetic resonance principle, T
2relaxation is determined by surface relaxation, and Surface Relaxation is relevant with media surface area, and Media Ratio surface the ratio of volume of voids V (the porous medium pore surface area S with) is larger, then relaxation is stronger, and vice versa, T
2surface is expressed as:
ρ in formula
2for T
2surface Relaxation intensity; (S/V)
holefor pore surface area and the ratio of volume of voids, then obtain T
2with the pass of aperture r be:
Fs is called geometrical form factors, and relevant with pore space size by the relaxation time of above formula visible hole inner fluid, hole is less, and specific area is larger, and the impact of surface interaction is stronger, T
2time is also shorter, relaxation time T
2be one to one with average pore size r, utilize T
2pore size and pore diameter distribution thereof are evaluated in distribution;
7th step, to the T that the 5th step inverting obtains
2area under spectrum is analyzed, nuclear magnetic resonance T2 T
2the integral area of spectrum to be proportional in sample contained fluid number, it is equal to or slightly less than the net porosity of sample, and the hole quantity in corresponding aperture is relevant with the size of peak area, after analyzing same sample difference soak time, T
2the change of area under spectrum and each peak proportion, obtain the change of cicada sample aperture gap volume, quantity;
8th step, the Magnetic resonance imaging result of the different soak time of same sample that the 5th step obtains is analyzed, intercept the cross section axially vertical with sample and carry out imaging, in image, black is background color, the region of turning white is hydrone region, what represent is aperture ranges, the brightness of image reflects the number of sample containing water amount, white speck is more, mean that sample hole is larger, otherwise, then hole is less, intuitively can find out the pore size distribution situation of sample inside like this, illustrate sample under hydration, the damage evolution process of inner structure.
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| CN106248712A (en) * | 2016-07-07 | 2016-12-21 | 中国石油大学(华东) | Seam method of making, the measuring method of microcrack density and the method for establishing model of microcrack and the preparation method of microcrack rock core in rock core |
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| CN105158288A (en) * | 2015-07-08 | 2015-12-16 | 上海大学 | Rapid detection method for magnetic interference of core on low-field nuclear magnetic resonance image |
| CN105241913A (en) * | 2015-10-10 | 2016-01-13 | 西安石油大学 | Nuclear magnetic resonance quantitative analysis method for rock micro-crack damage variable |
| CN107179232B (en) * | 2016-03-09 | 2020-03-27 | 中国石油化工股份有限公司 | Method for evaluating stability of shale |
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| CN106556616B (en) * | 2016-10-31 | 2017-12-12 | 重庆大学 | A kind of lower rock liquid nitrogen bursting by freezing crackle Visualization method of hydraulic pressure effect |
| CN106556616A (en) * | 2016-10-31 | 2017-04-05 | 重庆大学 | A kind of rock liquid nitrogen bursting by freezing crackle Visualization method under hydraulic pressure effect |
| CN106950242A (en) * | 2017-03-24 | 2017-07-14 | 西安石油大学 | A kind of method that quantitative assessment salinity influences on shale oil reservoir Absorb Water oil-displacement capacity |
| CN107561112A (en) * | 2017-09-23 | 2018-01-09 | 北京青檬艾柯科技有限公司 | A kind of magnetic nuclear resonance method for obtaining rock permeability section |
| CN108169099A (en) * | 2018-01-17 | 2018-06-15 | 西南石油大学 | A kind of shale gas RESERVOIR PORE STRUCTURE quantitative calculation method based on nuclear magnetic resonance |
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| CN112557277A (en) * | 2020-12-07 | 2021-03-26 | 北京科技大学 | Compact rock micropore connectivity identification classification evaluation method |
| CN112557277B (en) * | 2020-12-07 | 2022-03-25 | 北京科技大学 | Compact rock micropore connectivity identification classification evaluation method |
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| CN113405969A (en) * | 2021-06-22 | 2021-09-17 | 湖南工程学院 | Rock porosity evaluation method and system based on mineral ion concentration |
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