CN105067406A - Argon ion polishing/scanning electron microscope analyzing and sampling method for shale samples - Google Patents
Argon ion polishing/scanning electron microscope analyzing and sampling method for shale samples Download PDFInfo
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- CN105067406A CN105067406A CN201510497194.5A CN201510497194A CN105067406A CN 105067406 A CN105067406 A CN 105067406A CN 201510497194 A CN201510497194 A CN 201510497194A CN 105067406 A CN105067406 A CN 105067406A
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- shale
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Abstract
The invention discloses an argon ion polishing/scanning electron microscope analyzing and sampling method for shale samples including fragile shale core samples and rock debris samples. The method comprises steps of embedding, curing, cutting and polishing. By comparison with a traditional argon ion polishing/scanning electron microscope analyzing and sampling method, the analysis range of the samples is widened with the method, the shale core samples which are fragile in the cutting and sampling processes and the shale rock debris samples with smaller sizes can be analyzed, and meanwhile, the success rate of sampling is increased.
Description
Technical field
The present invention relates to field of petroleum geology, particularly a kind of argon ion polishing/SEM sample preparation method of shale samples.
Background technology
Scanning electron microscope is the important analysis research tool of oil geology industry, and it is in conjunction with argon ion polishing technology, can disclose the true micromechanism of shale inside, and a large amount of especially nanoscale is to micron-sized hole.These holes are most important for the occurrence status and the performance history in later stage studying shale gas.Before argon ion polishing is carried out to shale samples, need shale samples to be cut into suitable size (being generally 10mm × 10mm × 3mm), be then placed on baffle plate and adopt ar-ion beam to carry out polishing, as shown in Figure 1.
Therefore, the shale samples for argon ion polishing/scanning electron microscope analysis must meet certain size, is generally core sample, and not easily broken in cutting process.But because got shale core sample bedding or crack are comparatively grown, very easily broken due to the vibrations of cutting blade and washing away of chilled water when causing cutting it, be difficult to the bulk sample obtaining applicable polishing size; Or do not carry out in actual well drilled process getting core operation, cause the chip sample only having volume tiny can supply to analyze, but be difficult to its fixing cutting, and then argon ion polishing/scanning electron microscope analysis cannot be carried out to the shale samples of the above-mentioned type, thus obtain stratum microscopic information corresponding to these samples.
Summary of the invention
The object of this invention is to provide a kind of argon ion polishing/scanning electron microscope analysis method for making sample of shale samples.
To achieve these goals, the present invention is the mode utilizing embedding, is wrapped up by shale samples, is then cured it, cuts, polishing.On the one hand, frangible shale core sample wraps up by embedding medium, avoid the fracture phenomena caused by the unlatching of crack caused in cutting process, simultaneously due to the profile of embedded block comparatively rule, cutting times can be reduced to greatest extent, significantly improve the success ratio of argon ion polishing/scanning electron microscope analysis sample preparation.Another side, the shale chip sample of small volume after embedding solidification is equivalent to volume and increases, and it is little and irregular and be difficult to the shortcoming of fixing cutting to avoid volume.The present invention expands the sample analysis scope of argon ion polishing/scanning electron microscope effectively.
Argon ion polishing/scanning electron microscope analysis the method for making sample of frangible shale core of the present invention and shale chip sample comprises following processing step:
(1) embed: embedding medium is mixed according to certain ratio, remove bubble for subsequent use.Shale samples is placed in embedding plate, slowly adds embedding medium, and eliminate bubble.
(2) solidify: be statically placed in baking oven by the embedding plate being embedded with sample, heating at a certain temperature makes embedding medium solidify.
(3) the shale embedded samples after solidification is taken out from embedding plate, cut into the rectangular shape of rule with precision slicer, and ensure that the polishing section that needs of shale samples exposes.
(4) polishing: stick on baffle plate by the shale embedded samples of well cutting, is placed in argon ion polishing instrument and carries out polishing, can obtain the argon ion polishing shale samples being applicable to scanning electron microscopic observation and analyzing.
Described shale samples is frangible shale core sample or shale chip sample.
Described embedding medium is Eponate12 or other epoxy resin embedding mediums.
Described embedding medium Eponate12 composition is: resin monomer, dodecenylsuccinic anhydride (DDSA), N hydroxymethyl acrylamide (NMA), 2,4,6-tri-(dimethylamino methyl) phenol (DMP-30).Each several part ratio is: resin monomer/(DDSA+NMA)/DMP-30=1/0.69/0.01, wherein DDSA/NMA ratio is less than 0.3.
The mold shape of described embedding plate is the combination of rectangle, square, triangle or more shape.
Described solidification temperature is 40-80 DEG C, and set time is 12-24 hour.
Described polishing time is 3-6 hour.
Advantage of the present invention is mainly: investment is applied to shale samples process by the present invention first, reduces the requirement to shale samples profile and fragility.For frangible shale core sample, peripheral embedding medium effectively can prevent sample broke, and decreases cutting times, only once cuts and just can obtain polished surface, improve sample preparation success ratio.And for tiny shale chip sample, embedding medium solidification after, be equivalent to chip sample volume increase and more regular, be convenient to cutting operation.The present invention can expand the sample analysis scope of argon ion polishing/scanning electron microscope effectively.
Accompanying drawing explanation
Fig. 1 is shale samples argon ion polishing schematic diagram;
Fig. 2 is the argon ion polishing/SEM sample preparation step schematic diagram of frangible shale core sample.
Embodiment
Argon ion polishing/the SEM sample preparation of the frangible shale core sample of embodiment 1
As shown in Figure 2, the argon ion polishing/SEM sample preparation step of frangible shale core sample is as follows:
(1) embed: embedding medium Eponate12 is mixed according to the ratio of resin monomer/DDSA/NMA/DMP-30=1/0.2/0.49/0.01, remove bubble for subsequent use.Shale samples is placed in embedding plate, slowly adds the embedding medium configured, and eliminate bubble.
(2) solidify: the embedding plate being embedded with shale core sample is statically placed in baking oven, solidify 24 hours at 60 DEG C.
(3) cut: the shale core embedded samples after solidification is taken out from embedding plate, cut into the rectangular shape of rule with precision slicer, and ensure that the polishing section that needs of shale samples exposes.
(4) polishing: stick on baffle plate by the shale core embedded samples of well cutting, is placed in argon ion polishing instrument and carries out polishing 3 hours, can obtain the frangible shale core sample of argon ion polishing being applicable to scanning electron microscopic observation and analyzing.
Argon ion polishing/the SEM sample preparation of embodiment 2 shale chip sample
Argon ion polishing/SEM sample preparation the step of shale chip sample is as follows:
(1) embed: embedding medium Eponate12 is mixed according to the ratio of resin monomer/DDSA/NMA/DMP-30=1/0.1/0.59/0.01, remove bubble for subsequent use.Shale samples is placed in embedding plate, slowly adds the embedding medium configured, and eliminate bubble.
(2) solidify: the embedding plate being embedded with shale chip sample is statically placed in baking oven, solidify 16 hours at 60 DEG C.
(3) cut: the shale landwaste embedded samples after solidification is taken out from embedding plate, is placed in precision slicer, cut into the rectangular shape of rule, and ensure that the polishing section that needs of shale samples exposes.
(4) polishing: stick on baffle plate by the shale landwaste embedded samples of well cutting, is placed in argon ion polishing instrument and carries out polishing 3 hours, can obtain the argon ion polishing shale chip sample being applicable to scanning electron microscopic observation and analyzing.
Claims (8)
1. argon ion polishing/scanning electron microscope analysis method for making sample of shale samples, comprises embedding, solidification, cutting and polishing process.
2. the argon ion polishing/scanning electron microscope analysis method for making sample of a kind of shale samples according to claim 1, is characterized in that adopting following processing step:
(1) embed: configure embedding medium according to a certain percentage, then shale samples is placed in embedding plate, slowly add embedding medium, and eliminate bubble;
(2) solidify: the embedding plate being embedded with sample is placed in baking oven, heating makes embedding medium solidify;
(3) cut: the shale embedded samples after solidification is taken out from embedding plate, cut into the rectangular shape of rule with precision slicer, and ensure that the polishing section that needs of shale samples exposes;
(4) polishing: stick on baffle plate by the shale embedded samples of well cutting, is placed in argon ion polishing instrument and carries out polishing, can obtain the argon ion polishing shale samples being applicable to scanning electron microscopic observation and analyzing.
3. the argon ion polishing/scanning electron microscope analysis method for making sample of a kind of shale samples according to claim 1 and 2, is characterized in that: described shale samples is frangible shale core sample or shale chip sample.
4. the argon ion polishing/scanning electron microscope analysis method for making sample of a kind of shale samples according to claim 2, is characterized in that: the embedding medium adopted is Eponate12 or other epoxy resin embedding mediums.
5. the argon ion polishing/scanning electron microscope analysis method for making sample of a kind of shale samples according to claim 4, it is characterized in that: described embedding medium Eponate12 composition is: resin monomer, dodecenylsuccinic anhydride (DDSA), N hydroxymethyl acrylamide (NMA) and 2,4,6-tri-(dimethylamino methyl) phenol (DMP-30);
Each several part ratio is: resin monomer/(DDSA+NMA)/DMP-30=1/0.69/0.01, wherein the ratio of DDSA/NMA is less than 0.3.
6. the argon ion polishing/scanning electron microscope analysis method for making sample of a kind of shale samples according to claim 2, it is characterized in that: the solidification temperature adopted is 40-80 DEG C, set time is 12-24 hour.
7. the argon ion polishing/scanning electron microscope analysis method for making sample of a kind of shale samples according to claim 2, is characterized in that: the mold shape of the embedding plate adopted is the combination of rectangle, square, triangle or more shape.
8. the argon ion polishing/scanning electron microscope analysis method for making sample of a kind of shale samples according to claim 2, is characterized in that: the polishing time adopted is 3-6 hour.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105092897A (en) * | 2015-08-12 | 2015-11-25 | 北京泰瑞特检测技术服务有限责任公司 | Method of processing powder sample for argon ion beam cutting |
| CN105527117A (en) * | 2015-12-02 | 2016-04-27 | 成都理工大学 | Field in-situ sampling method for granular mixtures |
| CN105973674A (en) * | 2016-07-01 | 2016-09-28 | 中国科学院地质与地球物理研究所 | Preparation method of transmission electron microscope sample with large area of thin region |
| CN106842346A (en) * | 2016-12-23 | 2017-06-13 | 中国石油天然气股份有限公司 | The three-dimensional image forming apparatus and method of a kind of geologic reservoir |
| CN107620593A (en) * | 2017-08-08 | 2018-01-23 | 中国科学院地质与地球物理研究所 | Scanning system and method are considered to be worth doing with rock drilling in a kind of oil gas field scene |
| CN111474200A (en) * | 2020-04-16 | 2020-07-31 | 宸鸿科技(厦门)有限公司 | Method for preparing microstructure sample of electronic element |
| CN111595879A (en) * | 2019-02-21 | 2020-08-28 | 中国石油化工股份有限公司 | Multi-sample preparation device and method suitable for argon ion polishing |
| CN113125251A (en) * | 2019-12-31 | 2021-07-16 | 中国石油天然气集团有限公司 | Shale uniaxial creep test method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7663101B2 (en) * | 2006-05-22 | 2010-02-16 | Microscopy Innovations | System and methods for preparing microscopy samples |
| CN103808549A (en) * | 2014-03-11 | 2014-05-21 | 扬州大学 | Sample preparation method of scanning electron microscope of basalt fiber and asphalt mixed material fracture |
| CN104574420A (en) * | 2015-01-29 | 2015-04-29 | 中国石油大学(华东) | Nanoscale shale digital core building method |
-
2015
- 2015-08-14 CN CN201510497194.5A patent/CN105067406A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7663101B2 (en) * | 2006-05-22 | 2010-02-16 | Microscopy Innovations | System and methods for preparing microscopy samples |
| CN103808549A (en) * | 2014-03-11 | 2014-05-21 | 扬州大学 | Sample preparation method of scanning electron microscope of basalt fiber and asphalt mixed material fracture |
| CN104574420A (en) * | 2015-01-29 | 2015-04-29 | 中国石油大学(华东) | Nanoscale shale digital core building method |
Non-Patent Citations (4)
| Title |
|---|
| NATASHA ERDMAN: "Integrated Preparation and Imaging Techniques for the Microstructural and Geochemical Characterization of Shale by Scanning Electron Microscopy", 《ELECTRON MICROSCOPY OF SHALE HYDROCARBON RESERVOIRS:AAPG MEMOIR》 * |
| TED PELLA. INC.: "PELCO® Eponate 12™ Kit", 《PELCO TECHNICAL NOTES》 * |
| 王亮 等: "页岩的氩离子抛光制样研究", 《石油实验地质》 * |
| 黄新民: "《材料分析测试方法》", 31 January 2006 * |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105092897B (en) * | 2015-08-12 | 2017-12-26 | 北京泰瑞特检测技术服务有限责任公司 | A kind of processing method of powder sample for ar-ion beam cutting |
| CN105092897A (en) * | 2015-08-12 | 2015-11-25 | 北京泰瑞特检测技术服务有限责任公司 | Method of processing powder sample for argon ion beam cutting |
| CN105527117A (en) * | 2015-12-02 | 2016-04-27 | 成都理工大学 | Field in-situ sampling method for granular mixtures |
| CN105973674A (en) * | 2016-07-01 | 2016-09-28 | 中国科学院地质与地球物理研究所 | Preparation method of transmission electron microscope sample with large area of thin region |
| CN106842346B (en) * | 2016-12-23 | 2019-03-12 | 中国石油天然气股份有限公司 | A kind of three-dimensional image forming apparatus and method of geologic reservoir |
| CN106842346A (en) * | 2016-12-23 | 2017-06-13 | 中国石油天然气股份有限公司 | The three-dimensional image forming apparatus and method of a kind of geologic reservoir |
| CN107620593A (en) * | 2017-08-08 | 2018-01-23 | 中国科学院地质与地球物理研究所 | Scanning system and method are considered to be worth doing with rock drilling in a kind of oil gas field scene |
| US11041383B2 (en) | 2017-08-08 | 2021-06-22 | Institute Of Geology And Geophysics, Chinese Academy Of Sciences | System and method for scanning while-drilling rock fragments in an oil and gas field |
| CN111595879A (en) * | 2019-02-21 | 2020-08-28 | 中国石油化工股份有限公司 | Multi-sample preparation device and method suitable for argon ion polishing |
| CN111595879B (en) * | 2019-02-21 | 2023-02-10 | 中国石油化工股份有限公司 | Multi-sample preparation device and method suitable for argon ion polishing |
| CN113125251A (en) * | 2019-12-31 | 2021-07-16 | 中国石油天然气集团有限公司 | Shale uniaxial creep test method |
| CN111474200A (en) * | 2020-04-16 | 2020-07-31 | 宸鸿科技(厦门)有限公司 | Method for preparing microstructure sample of electronic element |
| CN111474200B (en) * | 2020-04-16 | 2023-09-26 | 宸鸿科技(厦门)有限公司 | Method for preparing microstructure sample of electronic element |
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