CN103323298A - Double piston type intact loess scanning electron microscope sample preparation method - Google Patents
Double piston type intact loess scanning electron microscope sample preparation method Download PDFInfo
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- CN103323298A CN103323298A CN 201310167512 CN201310167512A CN103323298A CN 103323298 A CN103323298 A CN 103323298A CN 201310167512 CN201310167512 CN 201310167512 CN 201310167512 A CN201310167512 A CN 201310167512A CN 103323298 A CN103323298 A CN 103323298A
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Abstract
The present invention discloses a double piston type intact loess scanning electron microscope sample preparation method, which has the following steps: 1, reagent preparation, wherein a soaking material is prepared from an epoxy resin, acetone, ethylenediamine and dibutyl phthalate, and is provided for soaking and curing a specimen; 2, infiltration device design, wherein an infiltration device comprises an upper piston, an upper portion bush, a lower portion bush and a lower piston, and a sealing state can be achieved after installation; and 3, specimen preparation and maintenance, wherein a soil taking device is adopted to take a intact loess specimen, and then is placed into a drying machine to dry until the mass is not changed, the soil taking device is taken out of the drying machine, the soaking material is added to the soil taking device in a dropwise manner so as to completely soak the specimen in the material, the piston is adopted to soak the specimen at a negative pressure environment, the soil taking device is stood on a test tube rack until the soaking material completely infiltrates the specimen, and the cured specimen is subjected to grinding and polishing so as to be used for electron microscope scanning. With the method, the specimen can be rapidly cured, the preparation has characteristics of miniaturization, standardization and batch property, and the specimen sampling position can be accurately considered.
Description
Technical field
The invention belongs to the technical field of geomaterial intact loess Study on Microstructure, especially relate to a kind of dual Piston intact loess scanning electron microscope example preparation method.
Background technology
In building and Geotechnical Engineering, collapsible loess has great harmfulness, and the Loess Collapsibility research on mechanism be unable to do without the research of loess microstructure.Current scanline Electron Microscopy and light microscope technique have been widely used in the research of geomaterial microstructure characteristic.In the past in the situation that lack advanced sample preparation means, have that the sample preparation time is long, the scope of application is narrow, can't mass, the problems such as miniaturization, standardization sample preparation.Therefore, how fast standardization, mass, standardization prepare the key that the scanning electron microscope test specimen is popularization scanning electron microscope micromechanism technology.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of method step simple and fast for above-mentioned deficiency of the prior art, can realize that standardization, miniaturization, mass prepare the scanning electron microscope test specimen.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of dual Piston intact loess scanning electron microscope example preparation method is characterized in that the method may further comprise the steps:
Step 1, test are prepared: with epoxy resin, acetone, ethylenediamine, dibutyl phthalate, be mixed with soak-out material;
Described soak-out material by epoxy resin, acetone, ethylenediamine, four kinds of materials of dibutyl phthalate take volume ratio as 100: 200: 7: 2 the preparation, this soak-out material has the advantages such as viscosity is little, the thermosetting performance is good;
The design of step 2, infiltration device:
Step 201, infiltration device are double-piston enclosure-type soil sample barrel, comprise upper piston (1), upper sleeve (2), lower sleeve portion (3) and lower piston (4);
Step 202, other equipment needed thereby instruments: dropper, 302 viscose glues, adhesive tape and test tube rack;
The preparation of step 3, test specimen and maintenance:
The position of step 301, selected required sampling;
Step 302, soil sample barrel upper sleeve blade-like one end (2-1) inwall is evenly smeared 302 viscose glues, be used for getting test specimen is fixed in the upper sleeve inwall, avoid the disturbance test specimen;
Step 303, soil sample barrel upper sleeve (2) is the selected sample position quick insertion of an end (2-1) alignment procedures 301 of blade-like, makes 2-5mm in the soil sample injection soil sample barrel, the test specimen sampling is finished;
Step 304, will be in the step 303 put into the baking oven baking after one hour with the soil sample barrel of test specimen, took out weighing every 10 minutes, until three weighing mass change are no more than 0.02g;
Step 305, lower sleeve portion (3) and upper sleeve (2) by helicitic texture (2-2) and (3-1) installed after inversion, make upper sleeve (2) and lower sleeve portion (3) junction be in sealing state, in case seepage when splashing into soaking solution;
Step 306, the soaking solution that step 1 is prepared splash on the test specimen of upper sleeve (2) from lower sleeve portion (3) with dropper, make soaking solution exceed test specimen 8-15mm, and test specimen is fully immersed in the soaking solution;
Step 307, the material for the treatment of step 1 preparation permeate test specimen fully and see through test specimen and flow into soil sample barrel upper sleeve (2) near after the piston part, and the soil sample barrel lower sleeve portion (3) of sealing is taken off, and pour out soak-out material;
Step 308, the cutting of the test specimen after will solidifying, grind, be used for electron-microscope scanning after the polishing.
Above-mentioned a kind of dual Piston intact loess scanning electron microscope example preparation method is characterized in that: the soaking solution described in the step 1 be epoxy resin, acetone, ethylenediamine, four kinds of materials of dibutyl phthalate take volume ratio as 100: 200: 7: 2 is formulated;
Above-mentioned a kind of dual Piston intact loess scanning electron microscope example preparation method, it is characterized in that: small-sized soil sample barrel described in the step 201 is comprised of upper piston (1), upper sleeve (2), lower sleeve portion (3) and lower piston (4), can reach sealing state after the instrument integral installation;
Above-mentioned a kind of dual Piston intact loess scanning electron microscope example preparation method is characterized in that: upper sleeve (2) one ends described in the step 201 are blade-like (2-1), in order to can finish easily and fast sampling when getting test specimen;
Above-mentioned a kind of dual Piston intact loess scanning electron microscope example preparation method is characterized in that: upper piston (1) external diameter is identical with upper sleeve (2) internal diameter in the infiltration device described in the step 201, can support the use;
Above-mentioned a kind of dual Piston intact loess scanning electron microscope example preparation method is characterized in that: lower piston (4) external diameter is identical with lower sleeve portion (3) internal diameter in the infiltration device described in the step 201, can support the use;
Above-mentioned a kind of dual Piston intact loess scanning electron microscope example preparation method, it is characterized in that: infiltration device middle and upper part sleeve (2) external diameter described in the step 201 is identical with lower sleeve portion (3) internal diameter, and upper sleeve (2) and lower sleeve portion (3) all have helicitic texture (2-2) and (3-1), upper sleeve (2) is connected 3 with lower sleeve portion) can pass through helicitic texture (2-2) and be connected 3-1) connect, finally make the inner one-tenth of soil sample barrel sealing state;
Above-mentioned a kind of dual Piston intact loess scanning electron microscope example preparation method, it is characterized in that: described in the step 202 in the required instrument, described dropper is used for soaking solution is splashed into soil sample barrel, and test tube rack is used for leaving standstill the small-sized soil sample barrel with test specimen and soaking solution;
Above-mentioned a kind of dual Piston intact loess scanning electron microscope example preparation method is characterized in that: the selected sampling desired position described in the step 301 is required soil body test specimen position of doing scanning electron microscope;
Above-mentioned a kind of dual Piston intact loess scanning electron microscope example preparation method, it is characterized in that: soaking solution is applied in soil sample barrel upper sleeve (2) inwall described in the step 302, the required inwall of smearing solution is the inwall of upper sleeve (2) blade-like port (2-1);
Above-mentioned a kind of dual Piston intact loess scanning electron microscope example preparation method, it is characterized in that: the specimen thickness of getting described in the step 303 is 2-5mm, available ruler is measured sampling thickness;
Above-mentioned a kind of dual Piston intact loess scanning electron microscope example preparation method, it is characterized in that: the baking test specimen described in the step 304 took out weighing every 10 minutes, until three weighing mass change are no more than 0.02g after one hour, purpose is to guarantee that test specimen reaches drying requirement, is convenient to solidify;
In sum, the invention discloses a kind of simple in structure, processing and fabricating and easy accessibility, use is easy to operate and result of use good, test result accurately, can soak into fast test specimen by easy realization solution, make test specimen be in solid state, and miniaturization, standardization, mass production are used for the method for the test specimen of scanning electron microscope.
The present invention compared with prior art has the following advantages:
1, simple in structure, the reasonable in design and processing and fabricating of the sampling equipment that adopts and easy accessibility, light small and exquisite, technique are simple and easy to produce.
2, upper sleeve (2) one ends of the used soil sample barrel of sampling are blade-like, the sampling mode fast and flexible.
3, use is easy and simple to handle, and soil sample is little, and undisturbed can realize that soaking solution infiltrates test specimen fast, makes test specimen reach fast solid state.
4, the whole parital vacuum technology that adopts of described soil sample barrel, the transparent material manufacturing is easy to actual instant observation.
5, because test material preparation mode Simple fast once can prepare a plurality of test specimens in batches, can carry out in batches the scanning electron microscope test.
6, can according to testing requirements, set in advance the test specimen sample position.
7, avoid the use of large-scale experiment chamber.
8, the test material preparation time is short.
Below by drawings and Examples, technical scheme of the present invention is described in further detail.
Description of drawings
Fig. 1 is overall schematic of the present invention.
Fig. 2 is soil sample barrel upper piston of the present invention (1) schematic diagram.
Fig. 3 is soil sample barrel upper sleeve of the present invention (2) schematic diagram.
Fig. 4 is soil sample barrel lower sleeve portion of the present invention (3) schematic diagram.
Fig. 5 is soil sample barrel lower piston of the present invention (4) schematic diagram.
Description of reference numerals:
The 1-upper piston; The 1-1-rubber structure; The 2-upper sleeve;
2-1-blade-like port; The 2-2-helicitic texture; The 3-lower sleeve portion;
The 3-1-helicitic texture; The 4-lower piston; The 4-1-rubber structure.
Embodiment
Embodiment 1
A kind of dual Piston intact loess scanning electron microscope example preparation method as shown in Figure 1 may further comprise the steps:
Step 1, test are prepared: with epoxy resin, acetone, ethylenediamine, dibutyl phthalate, be mixed with soak-out material;
Described soak-out material be epoxy resin, acetone, ethylenediamine, dibutyl phthalate take volume ratio as 100: 200: 7: 2 the preparation, this soak-out material has the advantages such as viscosity is little, the thermosetting performance is good;
Above-mentioned soaking solution be epoxy resin, acetone, ethylenediamine, four kinds of materials of dibutyl phthalate take volume ratio as 100: 200: 7: 2 is formulated;
The design of step 2, infiltration device:
Step 201, infiltration device are double-piston enclosure-type soil sample barrel, comprise upper piston (1), upper sleeve (2), lower sleeve portion (3) and lower piston (4);
Small-sized soil sample barrel described in the above-mentioned steps 201 is comprised of upper piston (1), upper sleeve (2), lower sleeve portion (3) and lower piston (4), can reach sealing state after the instrument integral installation; Described upper sleeve (2) one ends are blade-like, in order to can finish easily and fast sampling when getting test specimen;
Described upper piston (1) bottom is with rubber structure, and its external diameter is identical with described upper sleeve (2) internal diameter, can support the use and reach sealing effectiveness; Described lower piston (4) bottom is with rubber structure, and its external diameter is identical with described lower sleeve portion (3) internal diameter, can support the use;
Described upper sleeve (2) external diameter is identical with described lower sleeve portion (3) internal diameter, and upper sleeve (2) and lower sleeve portion (3) all have helicitic texture, upper sleeve (2) is connected 3 with lower sleeve portion) can connect by helicitic texture, finally make the inner one-tenth of soil sample barrel sealing state;
Step 202, other equipment needed thereby instruments: dropper, adhesive tape and test tube rack;
Above-mentioned stating in the required instrument, described dropper are used for soaking solution is splashed into soil sample barrel, and test tube rack is used for leaving standstill the small-sized soil sample barrel with test specimen and soaking solution;
The preparation of step 3, test specimen and maintenance:
Step 301, selected sampling desired position;
Above-mentioned selected sampling desired position is required soil body position of doing scanning electron microscope;
Step 302, with the soaking solution of the even smearing step of soil sample barrel inwall one preparation, be used for fixedly test specimen position, avoid the disturbance test specimen;
Above-mentioned soil sample barrel upper sleeve (2) inwall that soaking solution is applied in, the required inwall of smearing solution is the inwall of upper sleeve (2) blade-like one end;
Insert step 303, the selected positions of an end alignment procedures 301 that soil sample barrel upper sleeve (2) is blade-like, makes 2-5mm in the soil sample injection soil sample barrel, and the test specimen sampling is finished;
The specimen thickness of getting of the above is 2-5mm, and available ruler is measured sampling thickness;
Step 304, will be in the step 303 put into the baking oven baking after one hour with the soil sample barrel of test specimen, took out weighing every 10 minutes, until three weighing mass change are no more than 0.02g;
Above-mentioned baking test specimen took out weighing every 10 minutes after one hour, until three weighing mass change are no more than 0.02g, purpose is to guarantee that test specimen reaches drying requirement, is convenient to solidify;
Step 305, lower sleeve portion (3) and upper sleeve (2) are installed by helicitic texture, make upper sleeve (2) and lower sleeve portion (3) junction be in sealing state, in case seepage when splashing into soaking solution;
Step 306, the material that step 1 is prepared splash on the test specimen of upper sleeve (2) from lower sleeve portion (3) with dropper, make soaking solution exceed test specimen 8-15mm, and test specimen is fully immersed in the soaking solution;
Step 307, the material for the treatment of step 1 preparation permeate test specimen fully and see through test specimen and flow into soil sample barrel upper sleeve (2) near after the piston part, and the soil sample barrel lower sleeve portion (3) of sealing is taken off, and pour out soak-out material;
Step 308, the cutting of the test specimen after will solidifying, grind, be used for electron-microscope scanning after the polishing.
To sum up, simple in structure, the reasonable in design and processing and fabricating of sampling equipment of the present invention and easy accessibility, light small and exquisite, technique are simple and easy to produce, the sampling mode fast and flexible, use easy and simple to handle, soil sample is little, undisturbed, can realize that soaking solution infiltrates test specimen fast, make test specimen reach fast solid state, be easy to actual instant observation, can prepare in batches a plurality of test specimens, can carry out in batches the scanning electron microscope test, can set in advance the test specimen sample position, avoid the use of large-scale experiment chamber, the test material preparation time is short.
The above; it only is preferred embodiment of the present invention; be not that the present invention is imposed any restrictions, every any simple modification, change and equivalent structure of above embodiment being done according to the technology of the present invention essence changes, and all still belongs in the protection domain of technical solution of the present invention.
Claims (8)
1. dual Piston intact loess scanning electron microscope example preparation method, it is characterized in that the method may further comprise the steps: one, reagent is prepared: soak-out material is that epoxy resin, acetone, ethylenediamine, dibutyl phthalate are prepared jointly, is used for immersion, the curing of test specimen; Two, infiltrate the design of device: comprise upper piston (1), upper sleeve (2), lower sleeve portion (3) and lower piston (4), can reach sealing state after the installation; Three, the preparation of test specimen and maintenance: get the intact loess test specimen with soil sample barrel, the soil sample barrel that test specimen is housed is put into dryer to be baked to 10 minutes quality and no longer to change, after the taking-up soak-out material is splashed in the soil sample barrel, test specimen is fully immersed in the material, utilize upper piston (1) and lower piston (4) that test specimen is under the subnormal ambient and soak, soil sample barrel is statically placed on the test tube rack, until soak-out material infiltration test specimen, test specimen after soaking is ground and polishing, be used for electron-microscope scanning.
2. according to a kind of dual Piston intact loess scanning electron microscope example preparation method claimed in claim 1, it is characterized in that: the lower end of described upper piston (1) is used for reaching when it is installed in upper sleeve (2) sealing effectiveness with rubber structure (1-1).
3. according to claim 1 or 2 described a kind of dual Piston intact loess scanning electron microscope example preparation methods, it is characterized in that: upper sleeve (2) one ends are threaded structure (2-2), being used for it is connected with lower sleeve portion (3), the other end of described upper sleeve (2) is blade-like, can be fast when being convenient to take a sample, avoid the taking-up test specimen of disturbance.
4. according to a kind of dual Piston intact loess scanning electron microscope example preparation method claimed in claim 1, it is characterized in that: described lower sleeve portion (3) one ends are threaded structure (3-1), and this helicitic texture (3-1) supports the use with the helicitic texture (2-2) of claim 1 and 3 described upper sleeve (2).
5. according to the described a kind of dual Piston intact loess scanning electron microscope example preparation method of claim 1, it is characterized in that: described lower piston (4) lower end is used for reaching when it is installed in claim 1 and 4 described lower sleeve portion (3) sealing effectiveness with rubber structure.
6. according to a kind of dual Piston intact loess scanning electron microscope example preparation method claimed in claim 1, it is characterized in that: described soil sample barrel can reach sealing state after installing, be convenient to make test specimen to be issued to negative pressure state in the effect of double-piston, but curing solution rapid osmotic test specimen is finished solidification process;
7. according to a kind of dual Piston intact loess scanning electron microscope example preparation method claimed in claim 1, it is characterized in that: described curing soaking solution by epoxy resin, acetone, ethylenediamine, four kinds of materials of dibutyl phthalate take volume ratio as 100: 200: 7: 2 the preparation.
8. according to a kind of dual Piston intact loess scanning electron microscope example preparation method claimed in claim 7, it is characterized in that: the test specimen through solidifying after processing can be directly used in electron-microscope scanning after cutting, grinding, polishing.
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| CN 201310167512 CN103323298A (en) | 2013-05-08 | 2013-05-08 | Double piston type intact loess scanning electron microscope sample preparation method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104048980A (en) * | 2014-06-30 | 2014-09-17 | 西安科技大学 | Sample preparation and image acquisition method for analysis of micro structure of soil body |
| CN106526136A (en) * | 2017-01-04 | 2017-03-22 | 山东省水利科学研究院 | Liquid handling apparatus |
| CN109060417A (en) * | 2018-10-22 | 2018-12-21 | 长安大学 | A kind of original state coarse-grained soil sampling method |
-
2013
- 2013-05-08 CN CN 201310167512 patent/CN103323298A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104048980A (en) * | 2014-06-30 | 2014-09-17 | 西安科技大学 | Sample preparation and image acquisition method for analysis of micro structure of soil body |
| CN104048980B (en) * | 2014-06-30 | 2016-04-06 | 西安科技大学 | A kind of Soil Microstructure analysis sample preparation and image acquiring method |
| CN106526136A (en) * | 2017-01-04 | 2017-03-22 | 山东省水利科学研究院 | Liquid handling apparatus |
| CN109060417A (en) * | 2018-10-22 | 2018-12-21 | 长安大学 | A kind of original state coarse-grained soil sampling method |
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Application publication date: 20130925 |