CN106950231A - A kind of rock sample apparatus and method of use dual intensity micron CT quantitative judge rock forming minerals - Google Patents
A kind of rock sample apparatus and method of use dual intensity micron CT quantitative judge rock forming minerals Download PDFInfo
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Abstract
The present invention principally falls into petroleum gas and digital petrophysics field, is related specifically to a kind of rock sample apparatus and method of utilization dual intensity micron CT quantitative judge rock forming minerals.The rock sample device includes the standard specimen that rock sample and certain or a variety of rock sample components are constituted, and using dual intensity micron CT scan rock sample device and recognizes rock forming mineral using intensity slicing method.The present invention has sample preparation simple and sample nondestructive wound, the Minerals identification degree of accuracy is high, the characteristics of can embody mineral three-dimensional spatial distribution feature, solves prior art and recognizes shale minerals in the not high technical problem of the three dimensions degree of accuracy.
Description
Technical field
The present invention principally falls into petroleum gas and digital petrophysics field, is related specifically to a kind of micro- using dual intensity
The rock sample apparatus and method of rice CT quantitative judge rock forming minerals.
Background technology
In recent years, American technology, which breaks through, realizes the large-scale development of shale petroleum resources, changes Global Oil energy general layout.
China's shale oil gas resource reserve is ranked first in the world, and the areas such as the burnt masonry dam shale gas field in Sichuan Basin Fuling are realized at present
Commercialization exploitation, as the country that second is realized shale gas commercialization exploitation after the U.S., shale petroleum resources for
Chinese energy safety and stablize important role.Shale minerals are recognized and quantitative analysis is the evaluation of shale reservoir geology, dessert
Important content in prediction and hydraulic fracturing exploitation, accurately identifies simultaneously exploration of the energy quantitative analysis shale minerals for shale oil gas
Had great significance with exploitation.
At present, the main method to the Minerals identification in shale includes log analysis method（ECS, GEM, Flex etc.）, X penetrates
Line fluorescent element mud logging techniques（XRF）, X-ray diffraction total rock analytical technology（XRD）, light microscope identification, ensaying sweeps
Retouch the technologies such as Electronic Speculum, industry CT.Although recognizing that the means of shale minerals are many and each advantageous, there are many problems：Well logging
Technology can only obtain sampling interval larger one-dimensional data, and data volume is too small, without continuity；Light microscope and industry CT are known
Other shale minerals lack of resolution；Logging technique, XRF and ensaying ESEM do not have the reference of standard sample, pass through elder generation
There is certain error in the method that recognition element recombinates identification mineral again；Although ESEM resolution ratio is very high, two can only be obtained
Dimensional plane data, it is impossible to reflect shale minerals distributed in three dimensions feature；XRD, light microscope identification and ensaying ESEM
Sample making course is cumbersome and damage is caused to sample.
The above method has specific advantage, but there is also respective limitation, it is impossible to while realizing sample preparation not damaged, ore deposit
Thing recognition accuracy is high and characterizes these advantages of three-dimensional spatial distribution, it is necessary to which a kind of sample preparation is simple and sample nondestructive wound, mineral are known
The other degree of accuracy is high, can embody the shale minerals identification rock sample device and experimental method of mineral three-dimensional spatial distribution feature.
The content of the invention
In order to overcome the above-mentioned deficiencies of the prior art, it is an object of the invention to provide a kind of utilization dual-energy x-ray micron
CT（Also sometimes referred to as micron X-ray microscope or micron CT）The rock sample device and experimental method of shale minerals are recognized, is had
Sample preparation is simple and sample nondestructive wound, the Minerals identification degree of accuracy is high, the characteristics of can embody mineral three-dimensional spatial distribution feature, solves
Prior art recognizes shale minerals in the not high technical problem of the three dimensions degree of accuracy.
The present invention is achieved by the following technical solutions：
A kind of rock sample device of use dual intensity micron CT quantitative judge rock forming minerals, the rock sample device includes sample holder, rock-like
Product and standard specimen, the rock sample and standard specimen are placed in the sample holder；
The rock sample and standard specimen are full of the sample holder, it is ensured that rock sample and standard specimen are being contained when 360 degree of sample holder is rotated
Without skew in sample device；
The material selection gist of sample holder is X-ray through undamped after sample holder；It is described undamped for perfect condition, any material
Will have should be selected as far as possible in certain decay, experimentation the less material that decays to X-ray；
The component of the rock sample includes hole, a variety of organic matters, multiple gases and a variety of inanimate matters；The standard specimen according to
The compositional selecting of the rock sample, standard specimen is one in the hole, a variety of organic matters, multiple gases and a variety of inanimate matters
Plant or any a variety of mixing；
The rock can be any one in shale, sandstone, carbonate rock, metamorphic rock and volcanic rock.
Further, the size of the rock sample device is grade, and scope is 0.1 ~ 100mm.
Further, standard specimen includes inanimate matter, and inanimate matter standard specimen is pulverulence.
Further, the standard specimen includes the maximum mineral of the multi mineral Midst density.
Further, the rock is shale, and the standard specimen is quartz, carbonate rock and pyrite；Quartz granularity is 100
~ 200 mesh, pyrite granularity is 200 ~ 300 mesh, and carbonate rock includes calcite and dolomite, and granularity is 1000 ~ 1200 mesh.
Further, the sample holder is made up of polyimide tube and ab glue, and rock sample and standard specimen are placed in polyimides
In pipe, the two ends of polyimide tube are sealed by ab glue.
A kind of method of use dual intensity micron CT quantitative judge rock forming minerals, the described method comprises the following steps：
Dual intensity micron CT scan：The high-resolution for carrying out high energy and low energy respectively to rock sample device using X-ray micron CT devices is double
It can scan and obtain gray level image, high energy scanning voltage is 100 ~ 160kv, low energy scanning voltage is 40 ~ 100kv；
High-resolution is that each pixel size is micron level in image, and scope is 0.1 ~ 1000 μm；
The rock sample device includes rock sample to be measured and standard specimen, and the standard specimen is selected according to rock sample, selected from rock to be measured
One or more in sample component；
Gradation of image split plot design recognizes rock forming mineral：The high energy gray level image or low energy gray level image containing only rock are intercepted, is utilized
Intensity slicing method is directly partitioned into the maximum component of rock Midst density and the minimum component of density, is then identified using dual intensity method
True standard specimen mineral in rock.
Further, true standard specimen mineral are specially in dual intensity method identification rock：To high energy gray level image and low energy gray scale
Image carries out intensity slicing, intersecting calculate and obtains true standard specimen mineral in rock；
Low energy gray level image obtains mineral similar to standard specimen atomic number in rock；
High energy gray level image obtains mineral similar to standard specimen density in rock；
Low energy gray level image and high energy gray level image carry out etc. to location drawing picture is intersecting to be calculated, obtain in rock simultaneously with high energy mark
Sample and low energy standard specimen gray value all similar parts are true standard specimen mineral in rock.
Further, the size of the rock sample device is grade, and scope is 0.1 ~ 100mm, beneficial to high-precision scanning.
Further, swept in the standard specimen comprising the mineral that rock constituents Midst density is maximum beneficial to increase dual intensity micron CT
Retouch the contrast for obtaining gray scale image.
The Advantageous Effects of the present invention：
（1）Sample making is simple, and sample making course and data acquisition are to the equal not damaged of sample；
（2）Due to the rock sample loading device using small size, rock forming mineral high-resolution micron CT images can be obtained；
（3）Due to recognizing true mineral using dual intensity micron CT scan method and the reference of combination standard specimen, rock ore deposit is substantially increased
Recognition accuracy of the thing in three dimensions；
（4）Due to using appropriate gradation of image split plot design, shale can be divided into five major class mineral, shale minerals are improved
In the degree of accuracy of the identification of three dimensions；
（5）Due to using micron CT methods, the true three-dimension spatial distribution characteristic of rock forming mineral can be reflected.
Brief description of the drawings
Fig. 1, rock sample schematic device；
Fig. 2, dual intensity method recognize true mineral schematic diagram；
Fig. 3 a, original low energy gray-scale map；
Fig. 3 b, original high energy gray-scale map；
Fig. 4 a, low energy scanning tangent plane：Low energy recognizes mineral gray-scale map similar to carbonate rock atomic series；
Fig. 4 b, high energy scanning tangent plane：High energy recognizes mineral gray-scale map similar to carbonate rock density；
Fig. 4 c, Fig. 4 a and the intersecting calculating tangent planes of Fig. 4 b：True carbonate rock mineral gray-scale map；
Fig. 5 a, low energy scanning tangent plane：Low energy recognizes mineral gray-scale map similar to quartzy atomic series；
Fig. 5 b, high energy scanning tangent plane：High energy recognizes mineral gray-scale map similar to quartzy density；
Fig. 5 c, Fig. 5 a and the intersecting calculating tangent planes of Fig. 5 b：True quartz mineral gray-scale map；
Fig. 6 a, low energy scan original tangent plane；
Fig. 6 b, intensity slicing method recognize pyrite in Fig. 6 a；
Fig. 6 c, intensity slicing method recognize organic matter+hole in Fig. 6 a；
Fig. 6 d, dual intensity method recognize carbonate rock in Fig. 6 a；
Fig. 6 e, dual intensity method recognize quartzy in Fig. 6 a；
Fig. 6 f, intensity slicing method recognize Fig. 6 a CLAY MINERALS AND THEIR SIGNIFICANCEs+feldspar；
Fig. 6 g, shale minerals identification 2D figures；
Fig. 7, shale minerals identification 3D figures.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is explained in further detail.It should be appreciated that specific embodiment described herein is used only for explaining the present invention, and
It is not used in the restriction present invention.
On the contrary, the present invention covers any replacement done in the spirit and scope of the present invention being defined by the claims, repaiied
Change, equivalent method and scheme.Further, in order that the public has a better understanding to the present invention, below to the thin of the present invention
It is detailed to describe some specific detail sections in section description.Part without these details for a person skilled in the art
Description can also understand the present invention completely.
Embodiment 1
The present embodiment provides the rock sample device and experimental method of a kind of use dual intensity micron CT quantitative judge shale minerals, including rock sample
Device and experimental method.
Rock sample device is to include shale, three kinds of standard specimens（Quartz, carbonate rock and pyrite）, polyimide tube and ab glue
Small size rock sample loading device；
Experimental method includes dual intensity micron CT high resolution scannings, dual intensity method and recognizes true standard specimen mineral（Carbonate rock mineral and stone
English）With gradation of image split plot design identification shale minerals this three part, most at last shale be identified as quartz,（Organic matter+hole）、
（Clay mineral+feldspar）, carbonate rock and this five major class of pyrite and quantify the respective volumn concentration of calculating.
First, the preparation of rock sample device is carried out：Fig. 1 and for rock sample device schematic diagram, rock sample device comprising shale, three kinds
Standard specimen（Quartz, carbonate rock, pyrite）, polyimide tube and ab glue small size rock sample device.
Specifically, the shale in rock sample device is diameter 1mm cylinder；Three kinds of standard specimens are powder, stone in rock sample device
English granularity is 100 ~ 200 mesh, and pyrite granularity is 200 ~ 300 mesh, and carbonate rock includes calcite and dolomite, and granularity is 1000
~ 1200 mesh；The pipe that polyimide tube in rock sample device is wall thickness 0.5mm internal diameters 1.7mm.
Shale in rock sample device is located at the center of polyimide tube；Between shale and polyimide tube in rock sample device
Space by three kinds of standard specimens（Quartz, carbonate rock, pyrite）Dense pack, the gap not being filled with is air；Rock sample
Ab glues in device play a part of three kinds of standard specimen powder of seal rock sampling device and densification at the two ends of polyimide tube.
It should be noted that the shale in rock sample device is an application-specific, shale can also replace with sandstone, carbonic acid
The rocks such as rock salt, metamorphic rock and volcanic rock；Standard specimen in rock sample device is not limited to quartz, carbonate rock and pyrite, can also
Be other mineral such as organic matter, calcite, dolomite, mica, graphite, illite or shale, sandstone, carbonate rock,
The rock such as metamorphic rock and volcanic rock, it might even be possible to be the stream such as the gases such as air, nitrogen and water, oil.The shape of rock sample device is not
It is limited to cylinder, can also is the other shapes such as cuboid；The small size of rock sample device refers to grade, and scope is 0.1 ~ 100mm；
Standard specimen quantity is not limited to three, can be with any natural number.
Secondly, dual intensity micron CT scan experiment is carried out：Utilize current state-of-the-art micron CT devices（Zeiss Xradia
Versa 520）Gray level image is obtained to the high-resolution dual energy scan that the rock sample device prepared carries out high energy and low energy, high energy is swept
Voltage is retouched for 150kv, low energy scanning voltage is 50kv, resolution ratio is each 1.7 μm of pixel.High energy is not limited to X-ray energy
For 150kv, may be greater than 100kv, with Compton scattering act on based on energy range；Low energy is not limited to X-ray energy
50kv, can be less than 100kv, with photoelectric effect act on based on energy range；High-resolution is not limited in image each picture
Plain size is 1.7 μm, can be micron level, and scope is 0.1 ~ 1000 μm.
Then, true standard specimen mineral are recognized using dual intensity method（Carbonate rock mineral and quartz）：Utilize advanced graphics
As handling software to high energy and low energy gray level image progress intensity slicing and intersecting calculating, with standard specimen in acquisition shale（Carbonate
Rock or quartz）With standard specimen in the similar mineral of atomic number, shale（Carbonate rock or quartz）Density similar mineral and shale
In true standard specimen mineral（Carbonate rock or quartz）.
Specifically, illustrate with reference to Fig. 2, Fig. 3, Fig. 4 and Fig. 5, Fig. 2 is the schematic diagram that dual intensity method recognizes true mineral；Fig. 3
The original gradation figure obtained for dual energy scan, Fig. 3 a are that original low energy gray-scale map, Fig. 3 b are original high energy gray-scale map；Fig. 4 is double
Energy method recognizes the example of true carbonate rock mineral, and Fig. 4 a are carbonate rock mineral in low energy gray-scale map, and Fig. 4 b are high energy gray scale
Carbonate rock mineral in figure；Fig. 4 c are to calculate obtained true carbonate rock mineral by Fig. 4 a and Fig. 4 b are intersecting；Fig. 5 dual intensity methods
The example of true quartz mineral is recognized, Fig. 5 a are quartz mineral in low energy gray-scale map, and Fig. 5 b are quartz mineral in high energy gray-scale map；
Fig. 5 c are to calculate obtained true quartz mineral by Fig. 5 a and Fig. 5 b are intersecting.
Using 3-D view handle software low energy micron CT images are carried out in intensity slicing, selection shale with standard specimen（Carbon
Carbonate Rocks or quartz）The similar part of gray value, it is believed that be in shale with standard specimen（Carbonate rock or quartz）Atomic number is similar
Mineral（Such as Fig. 4 a and Fig. 5 a）；Software is handled to high energy micron CT image progress intensity slicings using 3-D view, selects page
With standard specimen in rock（Carbonate rock or quartz）The similar part of gray value, it is believed that be in shale with standard specimen（Carbonate rock or quartz）
The similar mineral of density (such as Fig. 4 b and Fig. 5 b)；Software is obtained to low energy and standard specimen is handled using 3-D view（Carbonate rock
Or quartz）The similar mineral of atomic number and high energy are obtained and standard specimen（Carbonate rock or quartz）The similar mineral of density, enter
The location drawing pictures such as row are intersecting to be calculated, it is believed that in shale simultaneously with high energy and low energy standard specimen（Carbonate rock or quartz）Gray value all phases
As partly be true standard specimen mineral（Carbonate rock or quartz）(such as Fig. 4 c and Fig. 5 c).
Finally, there was only shale using 3-D view processing software intercepts（Without standard specimen）High energy and low energy 3-D view,
Shale minerals are recognized using appropriate gradation of image split plot design, most at last shale be identified as quartz,（Organic matter+hole）、（Clay
Mineral+feldspar）, carbonate rock and this five major class of pyrite and quantify the respective volumn concentration of calculating.
Specifically, illustrate with reference to Fig. 6, Fig. 6 a are original low energy gray-scale map, Fig. 6 b are that gray level method recognizes pyrite, Fig. 6 c
Recognized for gray level method（Organic matter+hole）, Fig. 6 d are that dual intensity method recognizes carbonate rock, and Fig. 6 e are that dual intensity method recognizes quartz, Fig. 6 f
For（Clay mineral+feldspar）Identification.Gradation of image split plot design identification shale minerals are divided into three steps：1. utilize intensity slicing method
Directly be partitioned into pyrite and（Organic matter+hole）；2. identify carbonate rock mineral and quartz using dual intensity method；3. extract it
Remaining mineral, it is believed that be（Clay mineral+feldspar）.Final identification X-Y scheme is as shown in figure 6g.
It should be noted that using intensity slicing method be directly partitioned into pyrite and（Organic matter+hole）, it is because yellow iron
Ore deposit is the mineral of atom ordinal sum density maximum in shale, in gray level image（High energy or low energy）Middle gray value is maximum；（Organic matter
+ hole）For the mineral that atom ordinal sum density in shale is minimum, in gray level image（High energy or low energy）Middle gray value is minimum, profit
It is easy to be split with gradation of image split plot design.Recognize that true carbonate rock mineral percentage by volume is using dual intensity method
10.16%, the mineral percentage by volume similar to carbonate rock atomic number that wherein low energy is obtained is 12.11%, and high energy is obtained
The mineral percentage by volume similar to carbonate rock density be 19.82%.True quartz mineral volume hundred is recognized using dual intensity method
Fraction is 48.65%, and the mineral percentage by volume similar to quartzy atomic number that wherein low energy is obtained is 61.06%, and high energy is obtained
The mineral percentage by volume similar to quartzy density taken is 57.49%.Experimental method most at last shale be identified as quartz,（It is organic
Matter+hole）、（Clay mineral+feldspar）, carbonate rock and pyrite this five major class, percentage by volume is respectively 48.65%,
5.17%th, 34.94%, 10.16% and 1.08%, all results are 3 d image data, and 3 d image data can reflect
The true three-dimension spatial distribution characteristic of shale minerals, as shown in Figure 7.
Embodiment 2
The present embodiment is substantially the same manner as Example 1, and difference is, it is rectangular that rock sample is that shale in rectangle, rock sample device is located at
The side of shape polyimide tube, its complementary space places standard specimen.
Embodiment 3
The present embodiment is substantially the same manner as Example 1, and difference is that rock is sandstone, and standard specimen is the mineral such as quartz, feldspar；Or stone
Oil, water or other fluid；Or natural gas, CO2Deng gas.
Claims (10)
1. a kind of rock sample device of use dual intensity micron CT quantitative judge rock forming minerals, it is characterised in that the rock sample device includes
Sample holder, rock sample and standard specimen, the rock sample and standard specimen are placed in the sample holder；
The rock sample and standard specimen are full of the sample holder, it is ensured that rock sample and standard specimen are being contained when 360 degree of sample holder is rotated
Without skew in sample device；
The material selection gist of sample holder is X-ray through undamped after sample holder；
The component of the rock sample includes hole, a variety of organic matters, multiple gases and a variety of inanimate matters；The standard specimen according to
The compositional selecting of the rock sample, standard specimen is one in the hole, a variety of organic matters, multiple gases and a variety of inanimate matters
Plant or any a variety of mixing；
The rock can be any one in shale, sandstone, carbonate rock, metamorphic rock and volcanic rock.
2. a kind of rock sample device of use dual intensity micron CT quantitative judge rock forming minerals as claimed in claim 1, it is characterised in that institute
The size for stating rock sample device is grade, and scope is 0.1 ~ 100mm.
3. a kind of rock sample device of use dual intensity micron CT quantitative judge rock forming minerals as claimed in claim 1, it is characterised in that mark
Sample includes inanimate matter, and inanimate matter standard specimen is pulverulence.
4. a kind of rock sample device of use dual intensity micron CT quantitative judge rock forming minerals as claimed in claim 1, it is characterised in that institute
State standard specimen and include the maximum mineral of the multi mineral Midst density.
5. a kind of rock sample device of use dual intensity micron CT quantitative judge rock forming minerals as claimed in claim 1, it is characterised in that institute
Rock is stated for shale, the standard specimen is quartz, carbonate rock and pyrite；Quartz granularity is 100 ~ 200 mesh, and pyrite granularity is
200 ~ 300 mesh, carbonate rock includes calcite and dolomite, and granularity is 1000 ~ 1200 mesh.
6. a kind of rock sample device of use dual intensity micron CT quantitative judge rock forming minerals, its feature as described in claim 1-5 is any
It is that the sample holder is made up of polyimide tube and ab glue, and rock sample and standard specimen are placed in polyimide tube, polyimides
The two ends of pipe are sealed by ab glue.
7. a kind of method of use dual intensity micron CT quantitative judge rock forming minerals, it is characterised in that the described method comprises the following steps：
Dual intensity micron CT scan：The high-resolution for carrying out high energy and low energy respectively to rock sample device using X-ray micron CT devices is double
It can scan and obtain gray level image, high energy scanning voltage is 100 ~ 160kv, low energy scanning voltage is 40 ~ 100kv；
High-resolution is that each pixel size is micron level in image, and scope is 0.1 ~ 1000 μm；
The rock sample device includes rock sample to be measured and standard specimen, and the standard specimen is selected according to rock sample, selected from rock to be measured
One or more in sample component；
Gradation of image split plot design recognizes rock forming mineral：The high energy gray level image or low energy gray level image containing only rock are intercepted, is utilized
Intensity slicing method is directly partitioned into the maximum component of rock Midst density and the minimum component of density, is then identified using dual intensity method
True standard specimen mineral in rock.
8. a kind of method of use dual intensity micron CT quantitative judge rock forming minerals as claimed in claim 7, it is characterised in that dual intensity method
True standard specimen mineral are specially in identification rock：Intensity slicing, intersecting meter are carried out to high energy gray level image and low energy gray level image
Calculate and obtain true standard specimen mineral in rock；
Low energy gray level image obtains mineral similar to standard specimen atomic number in rock；
High energy gray level image obtains mineral similar to standard specimen density in rock；
Low energy gray level image and high energy gray level image carry out etc. to location drawing picture is intersecting to be calculated, obtain in rock simultaneously with high energy mark
Sample and low energy standard specimen gray value all similar parts are true standard specimen mineral in rock.
9. a kind of method of use dual intensity micron CT quantitative judge rock forming minerals as claimed in claim 7, it is characterised in that the rock
The size of sampling device is grade, and scope is 0.1 ~ 100mm, beneficial to high-precision scanning.
10. the method for a kind of use dual intensity micron CT quantitative judge rock forming minerals as claimed in claim 7, it is characterised in that described
Comprising the mineral that rock constituents Midst density is maximum in standard specimen, the contrast of gray scale image is obtained beneficial to increase dual intensity micron CT scan
Degree.
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