CN112033778A - Preparation method and system of micro sample of concrete interface transition zone - Google Patents
Preparation method and system of micro sample of concrete interface transition zone Download PDFInfo
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G01N1/00—Sampling; Preparing specimens for investigation
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- 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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- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
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- G01N23/203—Measuring back scattering
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G01N1/36—Embedding or analogous mounting of samples
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention relates to a preparation method and a system of a microscopic sample of a concrete interface transition zone, belonging to the field of civil engineering, wherein the method comprises the steps of preparing a square sample test piece for aggregate; grinding and polishing the square sample test piece and removing dust on the surface; placing the processed square aggregate sample test piece in a mould, and pouring the stirred cement paste on the sample test piece for vibration; curing the poured sample specimen under a sealed condition, and then demoulding; cutting a plurality of grooves with equal intervals along one edge on the surface of a sample test piece; cutting grooves with the same number and depth on the adjacent side; finally, cutting a row of aggregate sample strips on any side of the surface of the sample test piece; and (4) observing the shape of the prepared aggregate sample by a microscope by using the row of cut aggregate sample strips. The method well solves the problem that the concrete interface transition zone micro sample has no clear operation specification in the preparation process.
Description
Technical Field
The disclosure belongs to the field of civil engineering, and particularly relates to a preparation method and a system of a micro sample of a concrete interface transition area.
Background
The statements herein merely provide background related to the present disclosure and may not necessarily constitute prior art.
Because of low cost, high strength and good durability, the concrete is one of important building materials in civil engineering at present, and along with the large-scale use of the concrete, buildings have higher requirements on the performance of the concrete. The concrete building has prominent cracking and breakage problems in the production and service processes, which causes the durability problem of materials and even causes structural damage, the ratio of the tensile strength to the compressive strength of the concrete is small, and the concrete is typically brittle and easy to crack. Therefore, the scientific research aiming at the concrete cracking mechanism and the crack prevention and control rule has important significance for guiding the design of the durability and the crack resistance of the concrete and ensuring the engineering quality.
Therefore, how to control the crack resistance of concrete materials is always a key issue of interest in the industry. Because the research on the cracking mechanism of the micro-layer concrete is carried out on a micron level, the research on the aspect is mostly carried out through simulation due to the limitations of technologies and instruments, however, the results of the models are difficult to verify through tests, and the relationship between the concrete aggregate interface parameters and the macroscopic performance cannot be established.
BRIEF SUMMARY OF THE PRESENT DISCLOSURE
Aiming at the defects in the prior art, the present disclosure provides a method and a system for preparing a micro sample of a concrete interface transition zone.
At least one embodiment of the present disclosure discloses a method for preparing a micro sample of a transition zone of a concrete interface, the method comprising:
the method comprises the following steps: slicing the aggregate to prepare a square sample test piece; grinding and polishing the square sample test piece and removing dust on the surface;
step two: placing the square aggregate sample test piece treated in the step one in a mould, and pouring the stirred cement paste on the sample test piece for vibration; curing the poured sample test piece under a sealing condition for 28 days, and then demoulding;
step three: cutting off cement paste on the upper part of the test piece along the horizontal direction of the maintained test piece until the thickness of the cement paste on the surface of the aggregate is 0.2 mm; cutting a plurality of grooves with equal intervals along one edge on the surface of a sample test piece; cutting grooves with the same number and depth on the adjacent side; finally, cutting a row of aggregate sample strips on any side of the surface of the sample test piece;
step four: and observing the shape of the prepared aggregate sample by an electron microscope through the cut aggregate sample strips in the back row.
Further, the grinding in the first step is performed by using grinding discs with different particle sizes and mesh numbers, the upper surface and the lower surface of the aggregate sample test piece are ground and polished according to the particle size and mesh number descending sequence, and meanwhile, the ground and polished aggregate sample test piece is cleaned by using ultrasonic waves in an absolute ethyl alcohol environment.
Further, the mold in the second step is designed into a rectangular three-dimensional frame, the top of the rectangular three-dimensional frame is open, and the bottom and one side wall of the frame are detachable.
Further, the curing method in the second step adopts a plastic film or a curing film for sealing and curing.
Further, the fourth step is to examine the morphology of the prepared aggregate sample in a back-scattered electron mode by an Environmental Scanning Electron Microscope (ESEM).
At least one embodiment of the present disclosure also discloses a system for preparing a micro sample of a concrete interface transition zone, which comprises
A test sample manufacturing module: slicing the aggregate to prepare a square sample test piece; grinding and polishing the square sample test piece and removing dust on the surface; then placing the processed square aggregate sample test piece in a mould, and pouring the stirred cement paste on the sample test piece for vibration; curing the poured sample test piece under a sealing condition for 28 days, and then demoulding;
test sample cutting module: cutting off cement paste on the upper part of the test piece along the horizontal direction of the maintained test piece until the thickness of the cement paste on the surface of the aggregate is 0.2 mm; cutting a plurality of grooves with equal intervals along one edge on the surface of a sample test piece; cutting grooves with the same number and depth on the adjacent side; finally, cutting a row of aggregate sample strips on any side of the surface of the sample test piece;
test sample observation module: and (4) observing the shape of the prepared aggregate sample by a microscope by using the row of cut aggregate sample strips.
Further, in the test sample manufacturing module, grinding is performed by using grinding discs with different particle sizes and mesh numbers, grinding and polishing are performed on the upper surface and the lower surface of the aggregate sample test piece according to a particle size and mesh number descending sequence, and meanwhile, the ground and polished aggregate sample test piece is cleaned by using ultrasonic waves in an absolute ethyl alcohol environment.
Further, the mold in the test sample manufacturing module is designed into a rectangular three-dimensional frame, the top of the rectangular three-dimensional frame is open, and the bottom and one side wall of the frame are detachable.
Further, the maintenance method for manufacturing the module sample by the test sample adopts a plastic film or a maintenance film for sealing and maintenance.
Further, the test sample observation module is used for checking the morphology of the prepared aggregate sample in a back scattering electron mode through an environmental scanning electron microscope.
The beneficial effects of the above-mentioned this disclosure are as follows:
1) the preparation method of the concrete interface transition zone micro sample described in the disclosure well solves the problem that the concrete interface transition zone micro sample has no clear operation standard in the preparation process, and improves the sample quality by quantitatively determining the size of the micro sample, a maintenance system and a grinding and polishing process;
2) the preparation method disclosed by the invention is simple, the preparation precision is high, the cutting precision reaches 2-3 mu m, the preparation efficiency is high, dozens of micro samples can be prepared at one time, the difficulty in preparing the micro samples in the transition region of the concrete interface is reduced, the standardized production of the micro test samples in the transition region of the concrete interface is realized, and the quality of the test samples can be effectively ensured;
3) the design of the microscopic sample mold is also an important item in the preparation method, the cement paste belongs to a plastic material, the quality of the sample forming in the transition area is completely realized by the mold, and the design and the manufacture of the microscopic sample mold are the key for ensuring the quality of the sample;
4) the reliability of the quality of the microscopic sample is improved, the shape state of the microscopic sample can be accurately observed under a microscope, and the shape of the microscopic sample can be checked before testing.
Drawings
The accompanying drawings, which are included to provide a further understanding of the disclosure, illustrate embodiments of the disclosure and together with the description serve to explain the disclosure and are not to limit the disclosure.
Fig. 1 is a schematic view of a mold structure disclosed in at least one embodiment of the present disclosure;
FIG. 2 is a block diagram of a cured aggregate sample slice according to at least one embodiment of the present disclosure;
FIG. 3 is a schematic illustration of an aggregate sample slice cut through the aggregate sample slice in one direction on a surface of the aggregate sample slice as disclosed in at least one embodiment of the present disclosure;
FIG. 4 is a schematic illustration of an aggregate sample slice cut perpendicular to the cutting direction in FIG. 3 at the surface of the aggregate sample slice according to at least one embodiment of the present disclosure;
FIG. 5 is a schematic illustration of an aggregate strip cut from the surface of an aggregate sample slice according to at least one embodiment of the present disclosure;
fig. 6 is a schematic view of a blade cutting into aggregate at 20 μm according to at least one embodiment of the present disclosure.
Fig. 7 is a schematic view of a sample morphology under an Environmental Scanning Electron Microscope (ESEM) for a concrete micro-interface transition zone sample, in accordance with at least one embodiment of the present disclosure.
In the figure: 1. the device comprises a clamping groove, 2, an aggregate sheet, 3, hardened cement paste, 4, a blade, 5 and an aggregate and paste boundary.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this disclosure belongs.
In the description of the present disclosure, it is to be understood that the terms "upper", "lower", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are only for convenience in describing the present disclosure and simplifying the description, and do not indicate or imply that the referred devices or elements must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present disclosure.
The embodiment discloses a preparation method of a concrete interface transition zone microscopic sample, which comprises the following steps of aggregate thin slicing, stirring and pouring, sealing and maintaining, demolding and cutting, ESEM (electronic shelf life) morphology inspection and the like, wherein the concrete interface transition zone microscopic sample is prepared from P.O42.5 standard cement, quartzite aggregate and deionized water as required to be explained, a used instrument is a Struers Labopol-5 thin slicer, a cement paste stirrer, a plastic mold and a micro-cutter, and the water-cement ratio is 0.3.
(1) Slicing the aggregate by using a Struers Labopol-5 thin slicer, and slicing the thin aggregate slice into square slices with the thickness of 1cm multiplied by 1cm, wherein the damage of the slices to the aggregate is ignored;
(2) grinding, polishing and ultrasonically treating the aggregate sheet sample to remove dust on the aggregate sheet sample; polishing and grinding the upper surface and the lower surface of the cut aggregate sample slice in a descending order by using a disc with the granularity of 135-35 microns, and ultrasonically cleaning for 2-6min in an absolute ethyl alcohol environment;
(3) placing the polished aggregate thin slice at the bottom of a plastic mould shown in figure 1, casting the stirred cement paste (the water cement ratio is 0.3) at the top of the aggregate thin slice, placing the aggregate thin slice on a vibrating table for vibrating, and casting the aggregate thin slice with the thickness of 5 mm; the plastic mould is designed into a three-dimensional structure with the bottom surface of 1cm multiplied by 1cm and the height of 5mm, wherein the top of the mould is provided with an opening for placing the aggregate thin slices, the bottom of the mould and one of the side walls are detachable, and the bottom plate and one of the side walls of the mould are specifically clamped in through the clamping groove 1, so that the use is convenient, and the quality of a sample is ensured.
(4) Curing the poured sample test piece for 28 days under a sealed condition, and then demolding the aggregate sample; in order to prevent water loss, the microscopic sample maintenance method adopts a plastic film or a maintenance film for sealing maintenance.
(5) And as shown in figure 2, cutting the cured aggregate sample slice along the horizontal direction by using a micro cutting machine, cutting off the excess cement slurry 3 on the surface of the aggregate slice 2 until the slurry thickness on the surface of the aggregate is 0.2mm, so that the thickness of the whole thin slice sample is 1.2mm, and the cutting error is 2-3 μm.
(6) As shown in fig. 3, the cutting was performed along one side of a square in the direction perpendicular to the aggregate sample slice, the cutting pitch of the micro cutter was set to the sum of the width (100 μm) of the design cross section and the thickness of the blade, and the depth of the blade 4 cutting into the aggregate was 20 μm; the depth of the blade cutting into the aggregate is 20 mu m, so that a clear boundary between the aggregate and the slurry is ensured, and the test of the performance of the sample at the later stage is facilitated.
(7) As shown in FIG. 4, the cutting was performed along the other side of the square aggregate sample, and similarly, the cutting pitch of the micro cutter was set to the sum of the length (100 μm) of the cross section and the thickness of the blade, and the depth of the blade cutting into the aggregate was 20 μm.
(8) And as shown in fig. 5-6, cutting along any side of the square aggregate sample slice at a new interval of the cutting interval three times, and cutting a row of aggregate sample strips from the aggregate slice, namely obtaining the concrete interface transition zone micro sample. The cutting with the cutting distance of three times is to prevent the sample from being damaged by a blade in the cutting process, ensure the quality of the sample and reserve one row in three rows of samples.
(9) The prepared aggregate sample was examined for the morphology of the aggregate and slurry boundary 5 in a back-scattered electron (BSE) mode by an Environmental Scanning Electron Microscope (ESEM) as shown in fig. 7.
In addition, the embodiment of the disclosure also discloses a system for preparing the micro sample of the transition zone of the concrete interface, which mainly comprises
A test sample manufacturing module: prepared for preparing a prepared aggregate into a square sample test piece; grinding and polishing the square sample test piece and removing dust on the surface; placing the processed square aggregate sample test piece in a mould, and pouring the stirred cement paste on the sample test piece for vibration; curing the poured sample test piece under a sealing condition for 28 days, and then demoulding; the grinding in the test sample manufacturing module is performed by using grinding discs with different particle sizes and mesh numbers, the upper surface and the lower surface of the aggregate sample test piece are ground and polished according to the particle size and mesh number descending sequence, and meanwhile, the ground and polished aggregate sample test piece is cleaned by using ultrasonic waves in an absolute ethyl alcohol environment.
Test sample cutting module: the cement paste cutting device is prepared and used for cutting off cement paste on the upper part of a test piece along the horizontal direction of the cured test piece, and cutting a plurality of equally spaced grooves along one edge on the surface of the sample test piece; cutting grooves with the same number and depth on the adjacent side; cutting a row of aggregate sample strips on any side of the surface of a sample test piece; it should be noted that the mold in the test sample manufacturing module is designed into a rectangular three-dimensional frame, the top of the rectangular three-dimensional frame is open, and the bottom and one side wall of the frame are detachable; meanwhile, the maintenance method adopts a plastic film or a maintenance film for sealing and maintenance.
Test sample observation module: is prepared for inspecting the prepared aggregate sample morphology by an environmental scanning electron microscope in a back-scattered electron mode on the cut-out back row of aggregate sample strips.
Although the present disclosure has been described with reference to specific embodiments, it should be understood that the scope of the present disclosure is not limited thereto, and those skilled in the art will appreciate that various modifications and changes can be made without departing from the spirit and scope of the present disclosure.
Claims (10)
1. A preparation method of a microscopic sample of a concrete interface transition region is characterized by comprising the following steps:
the method comprises the following steps: slicing the aggregate to prepare a square sample test piece; grinding and polishing the square sample test piece and removing dust on the surface;
step two: placing the square aggregate sample test piece treated in the step one in a mould, and pouring the stirred cement paste on the sample test piece for vibration; curing the poured sample specimen under a sealed condition, and then demoulding;
step three: cutting off cement paste on the upper part of the test piece along the horizontal direction of the maintained test piece until the thickness of the cement paste on the surface of the aggregate is 0.2 mm; cutting a plurality of grooves with equal intervals along one edge on the surface of a sample test piece; cutting grooves with the same number and depth on the adjacent side; finally, cutting a row of aggregate sample strips on any side of the surface of the sample test piece;
step four: and (4) observing the shape of the prepared aggregate sample by a microscope by using the row of cut aggregate sample strips.
2. The method of claim 1, wherein the step of preparing the micro-scale sample of the concrete interface transition zone comprises: and C, grinding in the step I is carried out by using grinding discs with different particle sizes and mesh numbers, grinding and polishing the upper surface and the lower surface of the aggregate sample test piece according to a particle size and mesh number descending order, and meanwhile, the ground and polished aggregate sample test piece is cleaned by using ultrasonic waves in an absolute ethyl alcohol environment.
3. The method of claim 1, wherein the step of preparing the micro-scale sample of the concrete interface transition zone comprises: the mould in the second step is designed into a rectangular three-dimensional frame, the top of the rectangular three-dimensional frame is open, and the bottom and one side wall of the frame are detachable.
4. The method of claim 1, wherein the step of preparing the micro-scale sample of the concrete interface transition zone comprises: and in the second step, the maintenance method adopts a plastic film or a maintenance film for sealing and maintenance.
5. The method of claim 1, wherein the step of preparing the micro-scale sample of the concrete interface transition zone comprises: and fourthly, checking the morphology of the prepared aggregate sample in a back scattering electron mode through an environmental scanning electron microscope.
6. A preparation system of a concrete interface transition zone microscopic sample is characterized in that: comprises that
A test sample manufacturing module: prepared for preparing a prepared aggregate into a square sample test piece; grinding and polishing the square sample test piece and removing dust on the surface; placing the processed square aggregate sample test piece in a mould, and pouring the stirred cement paste on the sample test piece for vibration; curing the poured sample specimen under a sealed condition, and then demoulding;
test sample cutting module: cutting a plurality of grooves with equal intervals along one edge on the surface of a sample test piece; cutting grooves with the same number and depth on the adjacent side; cutting a row of aggregate sample strips on any side of the surface of a sample test piece;
test sample observation module: is prepared for observing the prepared aggregate sample shape by a microscope on the row of the aggregate sample strips after cutting.
7. The system for preparing a microscopic sample of a concrete interface transition zone according to claim 6, wherein: and grinding in the test sample manufacturing module is carried out by using grinding discs with different granularity and mesh numbers, grinding and polishing the upper surface and the lower surface of the aggregate sample test piece according to the granularity and mesh number descending order, and simultaneously, the ground and polished aggregate sample test piece is cleaned by using ultrasonic waves in an absolute ethyl alcohol environment.
8. The system for preparing a microscopic sample of a concrete interface transition zone according to claim 6, wherein: the mould in the test sample manufacturing module is designed into a rectangular three-dimensional frame, the top of the rectangular three-dimensional frame is open, and the bottom and one side wall of the frame are detachable.
9. The system for preparing a microscopic sample of a concrete interface transition zone according to claim 6, wherein: the maintenance method for manufacturing the module sample by the test sample adopts a plastic film or a maintenance film to carry out sealing maintenance.
10. The system for preparing a microscopic sample of a concrete interface transition zone according to claim 6, wherein: the test sample observation module is used for inspecting the form of the prepared aggregate sample in a back scattering electron mode through an environment scanning electron microscope.
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Cited By (1)
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| CN116577171A (en) * | 2023-06-02 | 2023-08-11 | 山东大学 | Method and system for evaluating and repairing interface transition zone based on phase hardness difference |
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| CN116577171A (en) * | 2023-06-02 | 2023-08-11 | 山东大学 | Method and system for evaluating and repairing interface transition zone based on phase hardness difference |
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