CN114088749B - Method and device for rapidly identifying broken quartz and biogenic quartz in shale - Google Patents
Method and device for rapidly identifying broken quartz and biogenic quartz in shale Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 418
- 239000010453 quartz Substances 0.000 title claims abstract description 416
- 230000000035 biogenic effect Effects 0.000 title claims abstract description 96
- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000013078 crystal Substances 0.000 claims abstract description 206
- 238000002050 diffraction method Methods 0.000 claims description 33
- 239000000203 mixture Substances 0.000 claims description 16
- 239000011435 rock Substances 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 12
- 238000004458 analytical method Methods 0.000 abstract description 20
- 238000012360 testing method Methods 0.000 abstract description 9
- 238000012545 processing Methods 0.000 abstract description 5
- 238000005553 drilling Methods 0.000 abstract description 4
- 238000004904 shortening Methods 0.000 abstract description 4
- 238000011068 loading method Methods 0.000 description 10
- 238000002441 X-ray diffraction Methods 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 238000005136 cathodoluminescence Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 2
- 239000003518 caustics Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 244000137852 Petrea volubilis Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 235000021185 dessert Nutrition 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000001239 high-resolution electron microscopy Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000007431 microscopic evaluation Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 238000004846 x-ray emission Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/05—Investigating materials by wave or particle radiation by diffraction, scatter or reflection
- G01N2223/056—Investigating materials by wave or particle radiation by diffraction, scatter or reflection diffraction
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/10—Different kinds of radiation or particles
- G01N2223/101—Different kinds of radiation or particles electromagnetic radiation
- G01N2223/1016—X-ray
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Abstract
The invention discloses a method and a device for rapidly identifying broken quartz and biogenic quartz in shale, wherein the method comprises the following steps: respectively obtaining diffraction intensity of a quartz 100 crystal face diffraction peak and diffraction intensity of a quartz 101 crystal face diffraction peak in a shale sample; calculating the ratio of the diffraction intensity of the diffraction peak of the quartz 100 crystal face to the diffraction intensity of the diffraction peak of the quartz 101 crystal face; comparing the ratio with a preset threshold; based on the comparison, the quartz in the shale sample is identified as either clastic quartz or biogenic quartz. The method for rapidly identifying the broken quartz and the biogenic quartz in the shale has the advantages of efficiently, rapidly and accurately identifying the quartz in the shale as the broken quartz or the biogenic quartz, avoiding the lengthy and inefficient analysis process of the traditional method, shortening the test period, improving the working efficiency, obviously saving the sample consumption of the drilling core, greatly shortening the sample processing period and obviously reducing the labor intensity of staff.
Description
Technical Field
The invention belongs to the technical field of oil and gas exploration and development, and particularly relates to a method and a device for rapidly identifying chipped quartz and biogenic quartz in shale.
Background
With the continuous deep practice of unconventional oil and gas exploration and development in China, resource evaluation of hydrocarbon source rock layers, particularly shale, is becoming an important content of exploration and research, and siliceous shale with high brittle mineral content is a preferable target layer of shale gas development due to the characteristics of high organic carbon, high porosity, high gas content and high compressibility. A great number of researches show that shale mainly containing biogenic silica often has higher quartz content, while shale mainly containing clastic quartz has relatively lower quartz content, but the cause identification work of quartz in shale, particularly in high-evolution shale, is difficult, so that the method capable of rapidly and effectively identifying the clastic quartz and the biogenic quartz in shale has very important significance for the exploration and development of shale gas.
At present, the method for identifying the quartz causes in shale still adopts the traditional geochemistry and mineralogy method, and mainly adopts an element comprehensive analysis method or a super-microscopic petrography method by means of high-resolution electron microscopy, cathodoluminescence and the like to carry out analysis for screening. The element comprehensive analysis method is mainly based on the identification analysis of the surplus elements, analyzes the amount of silicon elements above the Yu Liuyuan chip background, and identifies the silicon elements as biological cause siliceous. The supermicro petrography analysis method is to study the comprehensive characteristics of the quartz particles such as morphology and crystal form by electron microscopic observation combined energy spectrum analysis, and to judge the biological cause of siliceous and clastic quartz.
The main steps of the super microscopic analysis method include: 1) A small block of core sample having a diameter of about 1cm and a thickness of about 5mm was vertically core drilled with a small drill and a small hammer. 2) The deposit layer surface perpendicular to the sample was coarsely ground with a mechanical grinder and finely ground with fine sand paper. 3) And (5) primarily polishing the ground plane of the ground shale sample by using a rock fine grinding instrument. 4) The grinding plane is finely polished by a large-area ion polisher. 5) Based on observation of a scanning electron microscope, cathodoluminescence dotting test is carried out on different quartz particles to obtain cathodoluminescence images and spectrum results, and comprehensive analysis is carried out on the images and the results, so that the chip quartz and the biogenic quartz are more accurately judged.
The main steps of the element comprehensive analysis method comprise: 1) About 5g of small samples are selected, and crushed by a rock crusher until reaching 400 meshes. 2) The sample preparation is carried out by adopting a tabletting method, and the sample pressed into a wafer is clamped in a sample groove. 3) X-ray fluorescence spectrometry was performed. 4) The calculation is carried out by using an excessive silicon content calculation formula, wherein Si excess = Si sample- [ (Si/Al) background×Al sample ], (Si/Al) background adopts average shale ratio of 3.11, and the obtained percentage is the biogenic silicon percentage.
However, the existing two methods are high in labor intensity, high in test and analysis cost, long in sample processing and analysis period and large in required sample analysis quantity, and cannot meet the actual shale gas exploration requirements of 'dessert' layer determination, horizontal well design and fracturing scheme formulation, and a method capable of rapidly and effectively identifying crushed quartz and biogenic quartz in shale is needed.
Disclosure of Invention
The invention aims to provide a method capable of rapidly and effectively identifying chipped quartz and biogenic quartz in shale, and solves the problems of long sample treatment and analysis period and large sample analysis quantity in the prior art.
In view of the above, the invention provides a method and a device for rapidly identifying the crushed quartz and the biogenic quartz in the shale, which at least solve the problems of long sample treatment and analysis period and large sample analysis quantity.
In a first aspect, the invention provides a method for rapidly identifying chipped quartz and biogenic quartz in shale, comprising: respectively obtaining diffraction intensity of a quartz 100 crystal face diffraction peak and diffraction intensity of a quartz 101 crystal face diffraction peak in a shale sample; calculating the ratio of the diffraction intensity of the diffraction peak of the quartz 100 crystal face to the diffraction intensity of the diffraction peak of the quartz 101 crystal face; comparing the ratio with a preset threshold; and identifying quartz in the shale sample as clastic quartz or biogenic quartz according to a comparison result.
Optionally, the identifying quartz in the shale sample as clastic quartz or biogenic quartz according to the comparison result comprises: if the ratio is less than the preset threshold, quartz in the shale sample is clastic quartz; if the ratio is greater than the preset threshold, quartz in the shale sample is biogenic quartz; and if the ratio is equal to the preset threshold, quartz in the shale sample is a mixture of clastic quartz and biogenic quartz.
Optionally, performing powder diffraction analysis on the shale sample by using an X-ray diffractometer to obtain diffraction intensity of a quartz 100 crystal plane diffraction peak and diffraction intensity of a quartz 101 crystal plane diffraction peak in the shale sample.
Optionally, the quartz 100 crystal plane is a crystal plane with highest diffraction intensity of diffraction peaks in all crystal planes after diffraction analysis, and the quartz 101 crystal plane is a crystal plane with highest diffraction intensity of diffraction peaks in all crystal planes after diffraction analysis.
Optionally, the shale sample is a sample crushed by a rock crusher.
Optionally, the shale sample is loaded into the X-ray diffractometer by a sample positive loading method.
Optionally, the preset threshold value ranges from 0.2 to 0.3.
In a second aspect, the present invention also provides a device for rapidly identifying crushed quartz and biogenic quartz in shale, comprising: the diffraction intensity acquisition equipment is used for respectively acquiring diffraction intensity of a quartz 100 crystal face diffraction peak and diffraction intensity of a quartz 101 crystal face diffraction peak in the shale sample; a processor coupled to the diffraction intensity acquisition device, the processor performing the steps of: calculating the ratio of the diffraction intensity of the diffraction peak of the quartz 100 crystal face to the diffraction intensity of the diffraction peak of the quartz 101 crystal face; comparing the ratio with a preset threshold; and identifying quartz in the shale sample as clastic quartz or biogenic quartz according to a comparison result.
Optionally, the identifying quartz in the shale sample as clastic quartz or biogenic quartz according to the comparison result comprises: if the ratio is less than the preset threshold, quartz in the shale sample is clastic quartz; if the ratio is greater than the preset threshold, quartz in the shale sample is biogenic quartz; and if the ratio is equal to the preset threshold, quartz in the shale sample is a mixture of clastic quartz and biogenic quartz.
Optionally, the diffraction intensity obtaining device is an X-ray diffractometer, and the powder crystal diffraction analysis is performed on the shale sample by adopting the X-ray diffractometer to obtain the diffraction intensity of the quartz 100 crystal plane diffraction peak and the diffraction intensity of the quartz 101 crystal plane diffraction peak in the shale sample.
Optionally, the quartz 100 crystal plane is a crystal plane with highest diffraction intensity of diffraction peaks in all crystal planes after diffraction analysis, and the quartz 101 crystal plane is a crystal plane with highest diffraction intensity of diffraction peaks in all crystal planes after diffraction analysis.
Optionally, the shale sample is a sample crushed by a rock crusher.
Optionally, the shale sample is loaded into the X-ray diffractometer by a sample positive loading method.
Optionally, the preset threshold value ranges from 0.2 to 0.3.
The invention has the beneficial effects that: according to the method for rapidly identifying the broken quartz and the biogenic quartz in the shale, the diffraction intensity of the diffraction peak of the quartz 100 crystal face and the diffraction intensity of the diffraction peak of the quartz 101 crystal face are respectively obtained through the X-ray diffraction analysis of the shale sample, the ratio of the diffraction intensity of the diffraction peak of the quartz 100 crystal face to the diffraction intensity of the diffraction peak of the quartz 101 crystal face is compared with the preset threshold according to the difference of the crystal habit and the preferred orientation characteristics of different biogenic quartz, and the quartz in the shale is efficiently, rapidly and accurately identified as the broken quartz or the biogenic quartz according to the comparison result, so that the tedious and inefficient analysis process of the traditional method is avoided, the testing period is shortened, the working efficiency is improved, the sample consumption of a drilling rock core is obviously saved, the sample processing period is greatly shortened, the use and loss of chemical reagents are avoided, the environment is protected, and the labor intensity of workers is also obviously reduced.
The invention has other features and advantages which will be apparent from or are set forth in detail in the accompanying drawings and the following detailed description, which are incorporated herein, and which together serve to explain certain principles of the invention.
Drawings
The foregoing and other objects, features and advantages of the invention will be apparent from the following more particular descriptions of exemplary embodiments of the invention as illustrated in the accompanying drawings wherein like reference numbers generally represent like parts throughout the exemplary embodiments of the invention.
FIG. 1 illustrates a flow chart of a method for rapidly identifying rag quartz and biogenic quartz in shale in accordance with an embodiment of the present invention.
Fig. 2 illustrates a block diagram of an apparatus for rapidly identifying chip quartz and biogenic quartz in shale, according to an embodiment of the present invention.
Reference numerals illustrate:
102. diffraction intensity acquisition means; 104. a processor.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below. While the preferred embodiments of the present invention are described below, it should be understood that the present invention may be embodied in various forms and should not be limited to the embodiments set forth herein.
The invention provides a method for rapidly identifying chipped quartz and biogenic quartz in shale, which comprises the following steps: respectively obtaining diffraction intensity of a quartz 100 crystal face diffraction peak and diffraction intensity of a quartz 101 crystal face diffraction peak in a shale sample; calculating the ratio of the diffraction intensity of the diffraction peak of the quartz 100 crystal face to the diffraction intensity of the diffraction peak of the quartz 101 crystal face; comparing the ratio with a preset threshold; based on the comparison, the quartz in the shale sample is identified as either clastic quartz or biogenic quartz.
Specifically, a quartz 100 crystal face in the invention represents a quartz (100) crystal face in the field, a quartz 101 crystal face represents a quartz (101) crystal face in the field, and according to different crystal habits and preferred orientation characteristics of quartz with different causes, powder diffraction analysis is performed on a shale sample by adopting an X-ray diffraction technology to obtain diffraction intensity I 100 of a diffraction peak of the quartz 100 crystal face in the shale and diffraction intensity I 101 of a diffraction peak of the quartz 101 crystal face. Since the biogenic quartz has no obvious crystal form after recrystallization, the particle is not easy to generate preferred orientation, the relative intensity of diffraction peaks of two crystal faces of the biogenic quartz is good with the crystal form, and the chip quartz easy to preferred orientation is different, and further, according to statistics of the ratio of the diffraction intensity I 100 of diffraction peaks of a large number of known caustics of quartz 100 crystal faces to the diffraction intensity I 101 of diffraction peaks of quartz 101 crystal faces, a preset threshold value of the relative intensity ratio of the diffraction intensities of the two caustics of quartz is determined, and the ratio of the diffraction intensity I 100 of diffraction peaks of quartz 100 crystal faces to the diffraction intensity I 101 of diffraction peaks of quartz 101 crystal faces is compared with the preset threshold value, so that the effective and rapid identification of the chip quartz and the biogenic quartz in shale is realized.
According to the method for rapidly identifying the broken quartz and the biogenic quartz in the shale, the diffraction intensity of the diffraction peak of the quartz 100 crystal face and the diffraction intensity of the diffraction peak of the quartz 101 crystal face are respectively obtained through the X-ray diffraction analysis of the shale sample, the ratio of the diffraction intensity of the diffraction peak of the quartz 100 crystal face to the diffraction intensity of the diffraction peak of the quartz 101 crystal face is compared with a preset threshold according to the differences of the crystal habit and the preferential orientation characteristics of different biogenic quartz, and the quartz in the shale is efficiently, rapidly and accurately identified as the broken quartz or the biogenic quartz according to the comparison result, so that the tedious and inefficient analysis process of the traditional method is avoided, the testing period is shortened, the working efficiency is improved, the consumption of drilling core samples is obviously saved, the sample processing period is greatly shortened, the use and loss of chemical reagents are avoided, the environment is protected, and the labor intensity of workers is also obviously reduced.
Alternatively, identifying the quartz in the shale sample as clastic quartz or biogenic quartz based on the comparison results comprises: if the ratio is smaller than a preset threshold, quartz in the shale sample is clastic quartz; if the ratio is greater than a preset threshold, quartz in the shale sample is biogenic quartz; if the ratio is equal to the preset threshold, quartz in the shale sample is a mixture of clastic quartz and biogenic quartz.
Specifically, when the ratio of the diffraction intensity I 100 of the diffraction peak of the crystal face of the quartz 100 to the diffraction intensity I 101 of the diffraction peak of the crystal face of the quartz 101 is smaller than a preset threshold value, quartz in the shale sample is clastic quartz; when the ratio of the diffraction intensity I 100 of the diffraction peak of the crystal face of the quartz 100 to the diffraction intensity I 101 of the diffraction peak of the crystal face of the quartz 101 is larger than a preset threshold, quartz in the shale sample is biogenic quartz, and when the ratio of the diffraction intensity I 100 of the diffraction peak of the crystal face of the quartz 100 to the diffraction intensity I 101 of the diffraction peak of the crystal face of the quartz 101 is equal to the preset threshold, quartz in the shale sample is a mixture of clastic quartz and biogenic quartz.
As an alternative scheme, the powder diffraction analysis is carried out on the shale sample by adopting an X-ray diffractometer, and the diffraction intensity of the quartz 100 crystal face diffraction peak and the diffraction intensity of the quartz 101 crystal face diffraction peak in the shale sample are obtained.
Alternatively, the quartz 100 crystal plane is the crystal plane with the highest diffraction intensity of the diffraction peaks in all crystal planes after diffraction analysis, and the quartz 101 crystal plane is the crystal plane with the highest diffraction intensity of the diffraction peaks in all crystal planes after diffraction analysis.
Specifically, the shale is subjected to powder diffraction analysis by adopting an X-ray diffraction technology, a plurality of crystal faces of the shale are analyzed by adopting diffraction analysis, and a crystal face with the highest diffraction intensity of a diffraction peak is selected as a quartz 100 crystal face from analysis results of all crystal faces, and a crystal face with the highest diffraction intensity of the diffraction peak is selected as a quartz 101 crystal face.
Alternatively, the shale sample is a sample after comminution by a rock pulverizer.
For example, about 5g of small pieces of sample are selected, crushed by a rock crusher to 200 mesh, and the crushed sample is taken as shale sample.
Alternatively, shale samples are loaded into an X-ray diffractometer by a sample positive loading method.
Specifically, the sample is loaded in the sample holder of the X-ray diffractometer by adopting a normal loading method. The test is carried out according to SY/T5163-2010 standard, the instrument condition is set as a Cu target, the voltage of an X-ray tube is 40kV, the current is 100mA, the scanning speed is 4 degrees (2 theta)/min, and the scanning step width is 0.02 degrees (2 theta), so that diffraction analysis is carried out.
Alternatively, the preset threshold value ranges from 0.2 to 0.3.
Specifically, according to statistics of the ratio of the relative intensity I 100 of the quartz 100 crystal face diffraction peak and the relative intensity I 101 of the quartz 101 crystal face diffraction peak of a large number of known causative shale, the range limit value (preset threshold value) of the relative intensity ratio of the crystal face diffraction peaks of the two causative quartz is determined to be 0.2-0.3.
When the ratio of the diffraction intensity I 100 of the diffraction peak of the quartz 100 crystal face to the diffraction intensity I 101 of the diffraction peak of the quartz 101 crystal face is smaller than a preset threshold range, quartz in the shale sample is clastic quartz; when the ratio of the diffraction intensity I 100 of the diffraction peak of the crystal face of the quartz 100 to the diffraction intensity I 101 of the diffraction peak of the crystal face of the quartz 101 is larger than a preset threshold range, quartz in the shale sample is biogenic quartz, when the ratio of the diffraction intensity I 100 of the diffraction peak of the crystal face of the quartz 100 to the diffraction intensity I 101 of the diffraction peak of the crystal face of the quartz 101 is in the preset threshold range, quartz in the shale sample is a mixture of clastic quartz and biogenic quartz, when the ratio is close to 0.2, the clastic quartz is dominant, and when the ratio is close to 0.3, the biogenic quartz is dominant.
For example, when the ratio of the diffraction intensity I 100 of the diffraction peak of the crystal face of quartz 100 to the diffraction intensity I 101 of the diffraction peak of the crystal face of quartz 101 is smaller than a preset threshold range, and I 100/I101 is smaller than 0.2, quartz in the shale sample is clastic quartz; when the ratio of the diffraction intensity I 100 of the diffraction peak of the crystal face of the quartz 100 to the diffraction intensity I 101 of the diffraction peak of the crystal face of the quartz 101 is larger than a preset threshold range, quartz in the shale sample with I 100/I101 more than 0.3 is biogenic quartz; when the ratio of the diffraction intensity I 100 of the diffraction peak of the crystal face of quartz 100 to the diffraction intensity I 101 of the diffraction peak of the crystal face of quartz 101 is within a preset threshold range, I 100/I101 =0.23, quartz in the shale sample is a mixture of biogenic quartz and clastic quartz, and the clastic quartz is the main material.
The invention also provides a device for rapidly identifying the crushed quartz and the biogenic quartz in the shale, which comprises: the diffraction intensity acquisition equipment is used for respectively acquiring diffraction intensity of a quartz 100 crystal face diffraction peak and diffraction intensity of a quartz 101 crystal face diffraction peak in the shale sample; the processor is connected with the diffraction intensity acquisition device and executes the following steps: calculating the ratio of the diffraction intensity of the diffraction peak of the quartz 100 crystal face to the diffraction intensity of the diffraction peak of the quartz 101 crystal face; comparing the ratio with a preset threshold; based on the comparison, the quartz in the shale sample is identified as either clastic quartz or biogenic quartz.
Specifically, a quartz 100 crystal face in the invention represents a quartz (100) crystal face in the field, a quartz 101 crystal face represents a quartz (101) crystal face in the field, and according to different crystal habits and preferred orientation characteristics of quartz with different causes, powder diffraction analysis is performed on a shale sample by adopting an X-ray diffraction technology to obtain diffraction intensity I 100 of a diffraction peak of the quartz 100 crystal face in the shale and diffraction intensity I 101 of a diffraction peak of the quartz 101 crystal face. Since the biogenic quartz has no obvious crystal form after recrystallization, the particle is not easy to generate preferred orientation, the relative intensity of diffraction peaks of two crystal faces of the biogenic quartz is good with the crystal form, and the chip quartz easy to preferred orientation is different, and further, according to statistics of the ratio of the diffraction intensity I 100 of diffraction peaks of a large number of known biogenic quartz 100 crystal faces to the diffraction intensity I 101 of diffraction peaks of quartz 101 crystal faces, a preset threshold value of the relative intensity ratio of the diffraction peaks of the two biogenic quartz is determined, and according to comparison of the ratio of the diffraction intensity I 100 of diffraction peaks of quartz 100 crystal faces to the diffraction intensity I 101 of diffraction peaks of quartz 101 crystal faces with the preset threshold value, the effective and rapid identification of the chip quartz and the biogenic quartz in shale is realized.
According to the exemplary embodiment, the device for rapidly identifying the broken quartz and the biogenic quartz in the shale respectively obtains the diffraction intensity of the diffraction peak of the quartz 100 crystal face and the diffraction intensity of the diffraction peak of the quartz 101 crystal face through the X-ray diffraction analysis of the shale sample, compares the ratio of the diffraction intensity of the diffraction peak of the quartz 100 crystal face to the diffraction intensity of the diffraction peak of the quartz 101 crystal face with a preset threshold according to the differences of the crystallization habit and the preferential orientation characteristics of different biogenic quartz, and efficiently, rapidly and accurately identifies the quartz in the shale as the broken quartz or the biogenic quartz according to the comparison result, thereby avoiding the tedious and inefficient analysis process of the traditional method, shortening the test period, improving the working efficiency, obviously saving the consumption of drilling core samples, greatly shortening the sample processing period, avoiding the use and loss of chemical reagents, protecting the environment and obviously reducing the labor intensity of staff.
Alternatively, identifying the quartz in the shale sample as clastic quartz or biogenic quartz based on the comparison results comprises: if the ratio is smaller than a preset threshold, quartz in the shale sample is clastic quartz; if the ratio is greater than or equal to a preset threshold, the quartz in the shale sample is biogenic quartz.
Specifically, when the ratio of the diffraction intensity I 100 of the diffraction peak of the crystal face of the quartz 100 to the diffraction intensity I 101 of the diffraction peak of the crystal face of the quartz 101 is smaller than a preset threshold value, quartz in the shale sample is clastic quartz; when the ratio of the diffraction intensity I 100 of the diffraction peak of the crystal face of the quartz 100 to the diffraction intensity I 101 of the diffraction peak of the crystal face of the quartz 101 is larger than a preset threshold, quartz in the shale sample is biogenic quartz; if the ratio is equal to the preset threshold, quartz in the shale sample is a mixture of clastic quartz and biogenic quartz.
As an alternative scheme, the diffraction intensity obtaining device is an X-ray diffractometer, and powder crystal diffraction analysis is performed on the shale sample by adopting the X-ray diffractometer to obtain the diffraction intensity of the quartz 100 crystal plane diffraction peak and the diffraction intensity of the quartz 101 crystal plane diffraction peak in the shale sample.
Alternatively, the quartz 100 crystal plane is the crystal plane with the highest diffraction intensity of the diffraction peaks in all crystal planes after diffraction analysis, and the quartz 101 crystal plane is the crystal plane with the highest diffraction intensity of the diffraction peaks in all crystal planes after diffraction analysis.
Specifically, the shale is subjected to powder diffraction analysis by adopting an X-ray diffraction technology, a plurality of crystal faces of the shale are analyzed by adopting diffraction analysis, and a crystal face with the highest diffraction intensity of a diffraction peak is selected as a quartz 100 crystal face from analysis results of all crystal faces, and a crystal face with the highest diffraction intensity of the diffraction peak is selected as a quartz 101 crystal face.
Alternatively, the shale sample is a sample after comminution by a rock pulverizer.
For example, about 5g of small pieces of sample are selected, crushed by a rock crusher to 200 mesh, and the crushed sample is taken as shale sample.
Alternatively, shale samples are loaded into an X-ray diffractometer by a sample positive loading method.
Specifically, the sample is loaded in the sample holder of the X-ray diffractometer by adopting a normal loading method. The test is carried out according to SY/T5163-2010 standard, the instrument condition is set as a Cu target, the voltage of an X-ray tube is 40kV, the current is 100mA, the scanning speed is 4 degrees (2 theta)/min, and the scanning step width is 0.02 degrees (2 theta), so that diffraction analysis is carried out.
Alternatively, the preset threshold value ranges from 0.2 to 0.3.
When the ratio of the diffraction intensity I 100 of the diffraction peak of the quartz 100 crystal face to the diffraction intensity I 101 of the diffraction peak of the quartz 101 crystal face is smaller than a preset threshold range, quartz in the shale sample is clastic quartz; when the ratio of the diffraction intensity I 100 of the diffraction peak of the crystal face of the quartz 100 to the diffraction intensity I 101 of the diffraction peak of the crystal face of the quartz 101 is larger than a preset threshold range, quartz in the shale sample is biogenic quartz, when the ratio of the diffraction intensity I 100 of the diffraction peak of the crystal face of the quartz 100 to the diffraction intensity I 101 of the diffraction peak of the crystal face of the quartz 101 is in the preset threshold range, quartz in the shale sample is a mixture of clastic quartz and biogenic quartz, when the ratio is close to 0.2, the clastic quartz is dominant, and when the ratio is close to 0.3, the biogenic quartz is dominant.
For example, when the ratio of the diffraction intensity I 100 of the diffraction peak of the crystal face of quartz 100 to the diffraction intensity I 101 of the diffraction peak of the crystal face of quartz 101 is smaller than a preset threshold range, and I 100/I101 is smaller than 0.2, quartz in the shale sample is clastic quartz; when the ratio of the diffraction intensity I 100 of the diffraction peak of the crystal face of the quartz 100 to the diffraction intensity I 101 of the diffraction peak of the crystal face of the quartz 101 is larger than a preset threshold range, quartz in the shale sample with I 100/I101 more than 0.3 is biogenic quartz; when the ratio of the diffraction intensity I 100 of the diffraction peak of the crystal face of quartz 100 to the diffraction intensity I 101 of the diffraction peak of the crystal face of quartz 101 is within a preset threshold range, I 100/I101 =0.23, quartz in the shale sample is a mixture of biogenic quartz and clastic quartz, and the clastic quartz is the main material.
Example 1
FIG. 1 illustrates a flow chart of a method for rapidly identifying rag quartz and biogenic quartz in shale in accordance with an embodiment of the present invention.
As shown in fig. 1, the method for rapidly identifying the crushed quartz and the biogenic quartz in the shale comprises the following steps:
step 1: respectively obtaining diffraction intensity of a quartz 100 crystal face diffraction peak and diffraction intensity of a quartz 101 crystal face diffraction peak in a shale sample;
and carrying out powder diffraction analysis on the shale sample by adopting an X-ray diffractometer to obtain the diffraction intensity of the quartz 100 crystal plane diffraction peak and the diffraction intensity of the quartz 101 crystal plane diffraction peak in the shale sample.
The quartz 100 crystal plane is the crystal plane with the highest diffraction intensity of diffraction peaks in all crystal planes after diffraction analysis, and the quartz 101 crystal plane is the crystal plane with the highest diffraction intensity of diffraction peaks in all crystal planes after diffraction analysis.
Wherein the shale sample is a sample crushed by a rock crusher.
Wherein, shale samples are loaded in an X-ray diffractometer by a sampling normal loading method.
For example, about 5g of small samples are selected, and crushed by a rock crusher to 200 mesh. And (5) loading samples in a sample holder of the X-ray diffractometer by adopting a normal loading method. The test is carried out according to SY/T5163-2010 standard, instrument conditions: the diffraction analysis was performed on the Cu target, the X-ray tube voltage was 40kV, the current was 100mA, the scanning speed was 4 ° (2. Theta.)/min, and the scanning step width was 0.02 ° (2. Theta.).
Step 2: calculating the ratio of the diffraction intensity of the diffraction peak of the quartz 100 crystal face to the diffraction intensity of the diffraction peak of the quartz 101 crystal face;
step 3: comparing the ratio with a preset threshold;
wherein the preset threshold value ranges from 0.2 to 0.3.
Step 4: based on the comparison, the quartz in the shale sample is identified as either clastic quartz or biogenic quartz.
Wherein, according to the comparison result, identifying quartz in the shale sample as clastic quartz or biogenic quartz comprises: if the ratio is smaller than a preset threshold, quartz in the shale sample is clastic quartz; if the ratio is greater than a preset threshold, quartz in the shale sample is biogenic quartz; if the ratio is equal to the preset threshold, quartz in the shale sample is a mixture of clastic quartz and biogenic quartz.
For example, when the ratio of the diffraction intensity I 100 of the diffraction peak of the crystal face of quartz 100 to the diffraction intensity I 101 of the diffraction peak of the crystal face of quartz 101 is smaller than a preset threshold range, and I 100/I101 is smaller than 0.2, quartz in the shale sample is clastic quartz; when the ratio of the diffraction intensity I 100 of the diffraction peak of the crystal face of the quartz 100 to the diffraction intensity I 101 of the diffraction peak of the crystal face of the quartz 101 is larger than a preset threshold range, quartz in the shale sample with I 100/I101 more than 0.3 is biogenic quartz; when the ratio of the diffraction intensity I 100 of the diffraction peak of the crystal face of quartz 100 to the diffraction intensity I 101 of the diffraction peak of the crystal face of quartz 101 is within a preset threshold range, I 100/I101 =0.23, quartz in the shale sample is a mixture of biogenic quartz and clastic quartz, and the clastic quartz is the main material.
Example two
Fig. 2 illustrates a block diagram of an apparatus for rapidly identifying chip quartz and biogenic quartz in shale, according to an embodiment of the present invention.
As shown in fig. 2, the device for rapidly identifying the crushed quartz and the biogenic quartz in the shale comprises:
The diffraction intensity obtaining device 102 is used for respectively obtaining diffraction intensity of a quartz 100 crystal face diffraction peak and diffraction intensity of a quartz 101 crystal face diffraction peak in the shale sample;
a processor 104, the processor 104 being connected to the diffraction intensity acquisition device 102, the processor 104 performing the steps of: calculating the ratio of the diffraction intensity of the diffraction peak of the quartz 100 crystal face to the diffraction intensity of the diffraction peak of the quartz 101 crystal face; comparing the ratio with a preset threshold; based on the comparison, the quartz in the shale sample is identified as either clastic quartz or biogenic quartz.
Wherein, according to the comparison result, identifying quartz in the shale sample as clastic quartz or biogenic quartz comprises: if the ratio is smaller than a preset threshold, quartz in the shale sample is clastic quartz; if the ratio is greater than a preset threshold, quartz in the shale sample is biogenic quartz; if the ratio is equal to the preset threshold, quartz in the shale sample is a mixture of clastic quartz and biogenic quartz.
Wherein the preset threshold value ranges from 0.2 to 0.3.
For example, when the ratio of the diffraction intensity I 100 of the diffraction peak of the crystal face of quartz 100 to the diffraction intensity I 101 of the diffraction peak of the crystal face of quartz 101 is smaller than a preset threshold range, and I 100/I101 is smaller than 0.2, quartz in the shale sample is clastic quartz; when the ratio of the diffraction intensity I 100 of the diffraction peak of the crystal face of the quartz 100 to the diffraction intensity I 101 of the diffraction peak of the crystal face of the quartz 101 is larger than a preset threshold range, quartz in the shale sample with I 100/I101 more than 0.3 is biogenic quartz; when the ratio of the diffraction intensity I 100 of the diffraction peak of the crystal face of quartz 100 to the diffraction intensity I 101 of the diffraction peak of the crystal face of quartz 101 is within a preset threshold range, I 100/I101 =0.23, quartz in the shale sample is a mixture of biogenic quartz and clastic quartz, and the clastic quartz is the main material.
The diffraction intensity obtaining device 102 is an X-ray diffractometer, and performs powder diffraction analysis on the shale sample by adopting the X-ray diffractometer to obtain diffraction intensity of a quartz 100 crystal plane diffraction peak and diffraction intensity of a quartz 101 crystal plane diffraction peak in the shale sample.
The quartz 100 crystal plane is the crystal plane with the highest diffraction intensity of diffraction peaks in all crystal planes after diffraction analysis, and the quartz 101 crystal plane is the crystal plane with the highest diffraction intensity of diffraction peaks in all crystal planes after diffraction analysis.
Wherein the shale sample is a sample crushed by a rock crusher.
Wherein, shale samples are loaded in an X-ray diffractometer by a sampling normal loading method.
The foregoing description of embodiments of the invention has been presented for purposes of illustration and description, and is not intended to be exhaustive or limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the various embodiments described.
Claims (6)
1. A method for rapidly identifying crushed quartz and biogenic quartz in shale, comprising:
respectively obtaining diffraction intensity of a quartz 100 crystal face diffraction peak and diffraction intensity of a quartz 101 crystal face diffraction peak in a shale sample;
Calculating the ratio of the diffraction intensity of the diffraction peak of the quartz 101 crystal face to the diffraction intensity of the diffraction peak of the quartz 100 crystal face; the quartz 100 crystal face is the crystal face with highest diffraction intensity of diffraction peaks in all crystal faces after diffraction analysis, and the quartz 101 crystal face is the crystal face with high diffraction intensity of diffraction peaks in all crystal faces after diffraction analysis;
Comparing the ratio with a preset threshold, wherein the range of the preset threshold is 0.2 to 0.3;
identifying quartz in the shale sample as clastic quartz or biogenic quartz according to a comparison result;
wherein, according to the comparison result, identifying quartz in the shale sample as clastic quartz or biogenic quartz comprises:
If the ratio is less than 0.2, the quartz in the shale sample is clastic quartz;
if the ratio is greater than 0.3, the quartz in the shale sample is biogenic quartz;
If the ratio is between 0.2 and 0.3, the quartz in the shale sample is a mixture of clastic quartz and biogenic quartz.
2. The method for rapidly identifying the crushed quartz and the biogenic quartz in the shale according to claim 1, wherein the shale sample is subjected to powder diffraction analysis by an X-ray diffractometer to obtain the diffraction intensity of a quartz 100 crystal plane diffraction peak and the diffraction intensity of a quartz 101 crystal plane diffraction peak in the shale sample.
3. The method for rapid identification of chipped quartz and biogenic quartz in shale according to claim 2, wherein the shale sample is a sample after comminution by a rock pulverizer.
4. The method of rapidly identifying chipped quartz and biogenic quartz in shale of claim 3, wherein said shale sample is loaded in said X-ray diffractometer by a sample-and-load method.
5. A device for rapidly identifying crushed quartz and biogenic quartz in shale, comprising:
The diffraction intensity acquisition equipment is used for respectively acquiring diffraction intensity of a quartz 100 crystal face diffraction peak and diffraction intensity of a quartz 101 crystal face diffraction peak in the shale sample;
A processor coupled to the diffraction intensity acquisition device, the processor performing the steps of:
Calculating the ratio of the diffraction intensity of the diffraction peak of the quartz 101 crystal face to the diffraction intensity of the diffraction peak of the quartz 100 crystal face; the quartz 100 crystal face is the crystal face with highest diffraction intensity of diffraction peaks in all crystal faces after diffraction analysis, and the quartz 101 crystal face is the crystal face with high diffraction intensity of diffraction peaks in all crystal faces after diffraction analysis;
Comparing the ratio with a preset threshold, wherein the range of the preset threshold is 0.2 to 0.3;
identifying quartz in the shale sample as clastic quartz or biogenic quartz according to a comparison result;
wherein, according to the comparison result, identifying quartz in the shale sample as clastic quartz or biogenic quartz comprises:
If the ratio is less than 0.2, the quartz in the shale sample is clastic quartz;
if the ratio is greater than 0.3, the quartz in the shale sample is biogenic quartz;
If the ratio is between 0.2 and 0.3, the quartz in the shale sample is a mixture of clastic quartz and biogenic quartz.
6. The apparatus for rapid identification of crushed quartz and biogenic quartz in shale according to claim 5, wherein the diffraction intensity obtaining device is an X-ray diffractometer, and the X-ray diffractometer is used for performing powder diffraction analysis on the shale sample to obtain diffraction intensity of a quartz 100 crystal plane diffraction peak and diffraction intensity of a quartz 101 crystal plane diffraction peak in the shale sample.
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