CN111121646A - Method for detecting width of microcrack in transition zone of interface of reclaimed rubber concrete - Google Patents
Method for detecting width of microcrack in transition zone of interface of reclaimed rubber concrete Download PDFInfo
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Abstract
The invention discloses a method for detecting the width of microcracks in a transition zone of a reclaimed rubber concrete interface, which comprises the following steps: preparing a regenerated rubber concrete test piece, cutting a test piece by using a cutting machine, drying the test piece in a drying box to constant weight, vacuumizing and spraying gold on the surface, placing a small test piece after spraying the gold in a scanning electron microscope for observation, distinguishing different interfaces, selecting different magnification times to observe the test piece, photographing different interfaces of each group of test pieces, storing a picture in a computer, observing the appearance of an interface transition area, measuring the width of microcracks in the interface transition area, extracting the widths of the microcracks in the different interface transition areas, calculating the average width, the maximum and minimum value, the standard deviation and the variation coefficient of the microcracks, and calculating the width of the microcracks of the whole test piece. The method for detecting the width of the microcrack in the transition area of the interface of the recycled rubber concrete can be used for representing the width of the microcrack in the transition area of the interface of the recycled rubber concrete, and is high in precision, small in error and simple in test method.
Description
Technical Field
The invention belongs to the technical field of concrete crack detection, and relates to a method for detecting the width of a microcrack in a transition zone of a reclaimed rubber concrete interface.
Background
In recent ten years, research on cement-based materials has been developed rapidly, and the main characteristics are that the composition of concrete is more complicated and the functions are more diversified. The reclaimed rubber concrete has the advantages of good energy dissipation capacity, crack resistance, ductility, elastic shock absorption, sound insulation, noise reduction and the like as a novel engineering technology, can solve the problem of recycling of construction waste and waste tires, and has important significance for the sustainable development road of China.
The core of modern material science is the relationship between structure and performance, and the internal microstructure of the material determines various properties of the material. The Interface Transition Zone (ITZ) is the most important link for connecting cement slurry with completely different properties and aggregate materials into a whole and is the strength limit phase of concrete. When the environmental temperature and humidity change, due to the difference of the elastic modulus and the thermal expansion coefficient of the set cement and the aggregate, the set cement and the aggregate can generate uncoordinated deformation, so that local microcracks in an interface transition area are generated; the local water-cement ratio is relatively high due to the wall effect (wall effect) around the aggregate, and the local water-cement ratio also causes microcracks to be left in the transition area of the aggregate and cement paste interface, so that the microcracks become weak areas in concrete. Microcracks first initiate in the transition zone and are very prone to extend and propagate from this region into the set cement matrix, eventually leading to failure of the concrete structure. Therefore, in order to further reveal the microstructure characteristics of the ITZ of the reclaimed rubber concrete, the study on the ITZ microcrack width is very necessary.
In Chinese patent concrete crack detection method based on image distance transformation (application number: 201710983809.4, publication number: 108007355B), the method adopts a pixel gradient value symmetry analysis method, fully utilizes image distance transformation to reduce the calculated amount of crack connection, and has high calculation precision. But the calculation process is complex, the whole algorithm detection is based on the cracks in the concrete integral structure, and the situation of microcracks in the ITZ is not distinguished.
At present, the microstructure of the recycled aggregate concrete is researched by modern testing technology and instruments at home and abroad: microhardometer (VH), electron Scanning Electron Microscope (SEM), X-ray tomography (XRD), Nuclear Magnetic Resonance (NMR), electron energy spectrometer, mercury intrusion instrument (MIP), CT scan, and the like. The method mainly focuses on the research of the formation mechanism of the ITZ and the microscopic morphologies of the thickness, the hardness, the porosity, the crystal index and the like of the ITZ, but does not systematically research the influence of the size of the microcrack in the ITZ on the performance of a test piece, does not give a quantitative evaluation result on the width of the microcrack of the ITZ, and fails to objectively and accurately represent the microscopic characteristics of the interior of the concrete.
Disclosure of Invention
The invention aims to provide a method for detecting the width of the microcrack in the transition region of the interface of the recycled rubber concrete, which can represent the width of the microcrack in the transition region of the interface of the recycled rubber concrete and has the advantages of high precision, small error and simple test method.
The technical scheme adopted by the invention is that the method for detecting the width of the microcracks in the transition zone of the interface of the regenerated rubber concrete is implemented according to the following steps:
4, placing the small sample subjected to gold spraying in the step 3 in a scanning electron microscope for observation, finding a typical interface of the sample under a low-magnification condition, distinguishing different interfaces and numbering;
and 8, calculating the whole microcrack width of the test piece, and evaluating the mechanical property of the regenerated rubber concrete.
The present invention is also characterized in that,
and (3) the section of the sample in the step (2) contains an interface area of aggregate and cement paste, the surface of the section is relatively flat, and at least 3 samples are selected from each group of samples.
The step 3 specifically comprises the following steps:
step 3.1, placing the sample into a drying oven at 105 +/-5 ℃ for drying to constant weight, then clamping the sample by using tweezers, cleaning floating particles on the surface of the sample by using an air gun, and ensuring that the section is not disturbed when the sample is cleaned by using the air gun, so that the structure of the sample is consistent with that of the original sample;
and 3.2, firmly bonding the cleaned sample and the sample disc by using a conductive adhesive, then placing the sample disc into a gold plating device, setting the gold plating thickness to be 10nm, closing the top cover, vacuumizing, and carrying out gold spraying treatment on the surface of the sample, wherein the gold spraying lasts for 120 seconds each time until the set gold plating thickness is reached.
The step 4 specifically comprises the following steps:
the method comprises the steps of irradiating a sample for 10 minutes at a short distance by using a table lamp, observing the sample under a low-vacuum scanning electron microscope after a gold layer is solidified according to a light source of 3-5cm, adjusting and changing an observation area, observing at least 3 areas by using one sample, wherein each area comprises two interfaces of a rubber coarse aggregate-cement paste interface and a regenerated coarse aggregate-cement paste interface, finding a typical interface of the sample under a low-magnification condition, observing the typical interface by gradually magnifying the typical interface by multiple, distinguishing the two interfaces of the rubber coarse aggregate-cement paste interface and the regenerated coarse aggregate-cement paste interface, and numbering the two interfaces.
The step 5 specifically comprises the following steps:
each sample group is selected from 4 magnifications, namely four magnifications of 100 x, 2000 x, 5000 x and 10000 x are selected, 4 magnifications are taken for each interface, at least 24 photos are taken for one sample group, at least three samples are taken for each sample group, at least 24 x 3 pictures are taken for one sample group, 72 photos are taken for one sample group, and at least 72 x 4 pictures are taken for four sample groups, and the photos are stored in a computer.
The step 6 specifically comprises the following steps:
6.1, selecting an SEM picture which is clear in focus and has the resolution of at least 300 dpi/inch;
6.2, distinguishing areas of mortar, aggregate and interface transition areas in the picture;
step 6.3, scaling in the picture;
step 6.4, determining the width of the ITZ microcracks in the image by using the measurement function of the SEM;
6.5, selecting the measuring point space, wherein the crack length is l, and measuring every 1/3 l;
6.6, clicking a mouse to select a point in the picture, setting the point as a starting point, clicking the mouse to select another point, setting the point as a terminal point, and displaying the distance between the two points on the picture, namely the width of the microcrack at the point;
step 6.7, calculating the width of the microcrack: calculating a formula shown in formula (a);
wherein d isx(z)iIndicates the width of the micro-crack in the rubber coarse aggregate-cement paste interface or the recycled coarse aggregate-cement paste interface, wherein when d isx(z)iSubscript x, i.e. dxiShowing the microcrack width at the rubber coarse aggregate-cement slurry interface in the ith image when dx(z)iThe subscript being z, i.e. dziDenotes the microcrack width at the recycled coarse aggregate-cement slurry interface in the ith image, d1/3lDenotes the width of the microcrack at 1/3l, d2/3lDenotes the width of the microcrack at 2/3l, dlThe width of the microcracks at l is indicated.
The step 7 specifically comprises the following steps:
step 7.1, calculating the width of each crack in the transition area of each sample rubber coarse aggregate-cement paste interface and the regenerated coarse aggregate-cement paste interface respectively according to the step 6, averaging the cracks with all widths, and finally obtaining the average width of the cracks, wherein the calculation formula can be expressed as follows:
wherein m represents the number of SEM image analyses per sample, dx(z)iThe average microcrack width at the rubber coarse aggregate-cement slurry interface or recycled coarse aggregate-cement slurry interface in the ith image is shown, where i is 1, 2.. multidot.m,
the average microcrack width of the rubber coarse aggregate-cement paste interface or the regenerated coarse aggregate-cement paste interface is shown, and sigma represents summation operation;
step 7.2, respectively calculating the maximum microcrack width of the interface of the medium rubber coarse aggregate-cement paste or the interface of the regenerated coarse aggregate-cement paste:
dx(z),max＝max(dx(z)1,dx(z)2,dx(z)3......dx(z)m) (c)
wherein d isx(z),maxRepresents the maximum microcrack width in the rubber coarse aggregate-cement paste interface or the regenerated coarse aggregate-cement paste interface, and max () represents the operation of solving the maximum value;
step 7.3, respectively calculating the minimum microcrack width of the interface of the medium rubber coarse aggregate-cement paste or the interface of the regenerated coarse aggregate-cement paste:
dx(z),min＝min(dx(z)1,dx(z)2,dx(z)3......dx(z)m) (d)
wherein d isx(z),minRepresenting the minimum microcrack width in the rubber coarse aggregate-cement paste interface or the regenerated coarse aggregate-cement paste interface, and min () representing the minimum value solving operation;
step 7.4, respectively calculating the standard deviation of the interface of the medium rubber coarse aggregate-cement paste or the interface of the recycled coarse aggregate-cement paste:
wherein, σ represents a standard deviation,
representing root number opening operation;
step 7.5, respectively calculating the variation coefficient of the medium rubber coarse aggregate-cement paste interface or the regenerated coarse aggregate-cement paste interface:
wherein, CVRepresenting the coefficient of variation, and eliminating the data if the coefficient of variation is more than 15% during data statistical analysis.
The step 8 of calculating the whole microcrack width of the test piece specifically comprises the following steps:
wherein d represents the width of the whole microcracks, the content of the rubber coarse aggregate is α, the content of the recycled coarse aggregate is β, and d represents the total microcracksxiDenotes the microcrack width at the rubber coarse aggregate-cement slurry interface in the ith image, dziShowing the microcrack width at the recycled coarse aggregate-cement slurry interface in the ith image.
The invention has the advantages that
The method can utilize the existing resolution of SEM to the maximum extent, and represents the width of the micro-crack of the transition zone of the interface of the recycled rubber concrete by combining a statistical method, has high precision and small error, is simple in test method, greatly reduces the time consumed by image processing of concrete crack detection, can better evaluate the mechanical property of the concrete, and can be applied to the quality evaluation of concrete buildings which cannot be drilled and sampled in large sizes, such as hydraulic engineering dams, nuclear power station engineering, military protective structures and the like.
Drawings
FIG. 1 is a flow chart of a method of detecting the width of microcracks in a transition zone of a reclaimed rubber concrete interface according to the invention;
FIG. 2 is a schematic flow chart illustrating the operation of an embodiment of the method for detecting the width of the microcracks in the transition zone of the reclaimed rubber concrete interface according to the invention;
FIG. 3 is a schematic diagram of a concrete sample scanning sample and crack width extraction in an embodiment of a method for detecting the width of micro cracks in a transition zone of a reclaimed rubber concrete interface according to the present invention;
FIG. 4 is a graph showing the relationship between the width of the micro-crack and the compressive strength of the recycled rubber concrete in the embodiment of the method for detecting the width of the micro-crack in the transition zone of the interface of the recycled rubber concrete.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention discloses a method for detecting the width of microcracks in a transition zone of a reclaimed rubber concrete interface, which has a flow shown in figure 1 and is implemented according to the following steps:
step 3.1, placing the sample into a drying oven at 105 +/-5 ℃ for drying to constant weight, then clamping the sample by using tweezers, cleaning floating particles on the surface of the sample by using an air gun, and ensuring that the section is not disturbed when the sample is cleaned by using the air gun, so that the structure of the sample is consistent with that of the original sample;
step 3.2, firmly bonding the cleaned sample and the sample disc by using a conductive adhesive, then placing the sample disc into a gold plating device, setting the gold plating thickness to be 10nm, closing the top cover, vacuumizing, and carrying out gold spraying treatment on the surface of the sample, wherein the gold spraying lasts for 120 seconds each time until the set gold plating thickness is reached;
4, placing the small sample subjected to gold spraying in the step 3 in a scanning electron microscope for observation, finding a typical interface of the sample under a low-magnification condition, distinguishing different interfaces and numbering; the method specifically comprises the following steps:
irradiating the sample with a table lamp for 10 minutes at a short distance, observing the sample under a low-vacuum scanning electron microscope after a gold layer is solidified according to a light source of 3-5cm, adjusting and changing an observation area, observing at least 3 areas by one sample, wherein each area comprises two interfaces of a rubber coarse aggregate-cement paste interface and a regenerated coarse aggregate-cement paste interface, finding a typical interface of the sample under a low-magnification condition, observing the typical interface by gradually magnifying the typical interface, distinguishing the two interfaces of the rubber coarse aggregate-cement paste interface and the regenerated coarse aggregate-cement paste interface, and numbering the two interfaces;
selecting 4 magnification factors for each group of samples, namely selecting four factors of 100X, 2000X, 5000X and 10000X, taking 4 times for each interface, wherein at least 24 photos are taken for one sample, at least three samples are taken for each group of samples, at least 24X 3 is taken as 72 photos for one group of samples, and at least 72X 4 is taken as 288 photos for four groups of samples, and storing the photos in a computer;
6.1, selecting an SEM picture which is clear in focus and has the resolution of at least 300 dpi/inch;
6.2, distinguishing areas of mortar, aggregate and interface transition areas in the picture;
step 6.3, scaling in the picture;
step 6.4, determining the width of the ITZ microcracks in the image by using the measurement function of the SEM;
6.5, selecting the measuring point space, wherein the crack length is l, and measuring every 1/3 l;
6.6, clicking a mouse to select a point in the picture, setting the point as a starting point, clicking the mouse to select another point, setting the point as a terminal point, and displaying the distance between the two points on the picture, namely the width of the microcrack at the point;
step 6.7, calculating the width of the microcrack: calculating a formula shown in formula (a);
wherein d isx(z)iIndicates the width of the micro-crack in the rubber coarse aggregate-cement paste interface or the recycled coarse aggregate-cement paste interface, wherein when d isx(z)iSubscript x, i.e. dxiShowing the microcrack width at the rubber coarse aggregate-cement slurry interface in the ith image when dx(z)iThe subscript being z, i.e. dziDenotes the microcrack width at the recycled coarse aggregate-cement slurry interface in the ith image, d1/3lDenotes the width of the microcrack at 1/3l, d2/3lDenotes the width of the microcrack at 2/3l, dlRepresents the width of the microcracks at l;
step 7.1, calculating the width of each crack in the transition area of each sample rubber coarse aggregate-cement paste interface and the regenerated coarse aggregate-cement paste interface respectively according to the step 6, averaging the cracks with all widths, and finally obtaining the average width of the cracks, wherein the calculation formula can be expressed as follows:
wherein m represents the number of SEM image analyses per sample, dx(z)iThe average microcrack width at the rubber coarse aggregate-cement slurry interface or recycled coarse aggregate-cement slurry interface in the ith image is shown, where i is 1, 2.. multidot.m,
the average microcrack width of the rubber coarse aggregate-cement paste interface or the regenerated coarse aggregate-cement paste interface is shown, and sigma represents summation operation;
step 7.2, respectively calculating the maximum microcrack width of the interface of the medium rubber coarse aggregate-cement paste or the interface of the regenerated coarse aggregate-cement paste:
dx(z),max＝max(dx(z)1,dx(z)2,dx(z)3......dx(z)m) (c)
wherein d isx(z),maxRepresents the maximum microcrack width in the rubber coarse aggregate-cement paste interface or the regenerated coarse aggregate-cement paste interface, and max () represents the operation of solving the maximum value;
step 7.3, respectively calculating the minimum microcrack width of the interface of the medium rubber coarse aggregate-cement paste or the interface of the regenerated coarse aggregate-cement paste:
dx(z),min＝min(dx(z)1,dx(z)2,dx(z)3......dx(z)m) (d)
wherein d isx(z),minRepresenting the minimum microcrack width in the rubber coarse aggregate-cement paste interface or the regenerated coarse aggregate-cement paste interface, and min () representing the minimum value solving operation;
step 7.4, respectively calculating the standard deviation of the interface of the medium rubber coarse aggregate-cement paste or the interface of the recycled coarse aggregate-cement paste:
wherein, σ represents a standard deviation,
representing root number opening operation;
step 7.5, respectively calculating the variation coefficient of the medium rubber coarse aggregate-cement paste interface or the regenerated coarse aggregate-cement paste interface:
wherein, CVRepresenting the coefficient of variation, and eliminating the data if the coefficient of variation is more than 15% during data statistical analysis;
step 8, calculating the whole microcrack width of the test piece, and evaluating the mechanical property of the regenerated rubber concrete, wherein the step of calculating the whole microcrack width of the test piece specifically comprises the following steps:
wherein d represents the width of the whole microcracks, the content of the rubber coarse aggregate is α, the content of the recycled coarse aggregate is β, and d represents the total microcracksxiDenotes the microcrack width at the rubber coarse aggregate-cement slurry interface in the ith image, dziShowing the microcrack width at the recycled coarse aggregate-cement slurry interface in the ith image.
Example (b):
a method for detecting the width of microcracks in a transition zone of a reclaimed rubber concrete interface is shown in a flow chart of figures 1-2 and specifically comprises the following steps:
The raw materials for preparing the regenerated rubber concrete are determined according to the standard of the test method for the mechanical properties of the ordinary concrete (GB/T50081-2002) and the standard of the test method for the long-term performance and the durability of the ordinary concrete (GB/T50082-2009): cement, recycled coarse aggregate, rubber coarse aggregate, sand, water, an air entraining agent and a water reducing agent, and preparing a recycled rubber concrete test piece of 100mm multiplied by 100mm, wherein the rubber equal volume replaces part of the recycled coarse aggregate, and the recycled rubber concrete test piece is demoulded after standard curing to a specified age by matching with the formula shown in Table 1.
TABLE 1 compounding ratio of reclaimed rubber concrete
And 2, cutting the reclaimed rubber concrete test piece into small test pieces with the thickness not more than 15mm and the side length of 20mm multiplied by 20mm by using a cutting machine, wherein the section of each test piece must contain an interface area of aggregate and cement paste, the surface to be observed is smooth, at least 3 concrete test pieces in each group are selected, and a plurality of concrete test pieces are observed.
The method comprises the steps of sawing two parallel sections perpendicular to an interface where concrete cement paste and aggregate are bonded by a cutting machine to obtain a sample with the thickness smaller than 15mm and the side length of 20mm multiplied by 20mm and containing ITZ, and cutting off the vertical flat section and the bonding interface by a sharp edge to obtain a natural section of the sample containing an interface transition area, wherein the surface to be observed is smooth as much as possible, no overlarge mutation exists, and the imaging gray level change is ensured to be within a reasonable range.
And 3, placing the sample in a drying oven to be dried to constant weight, removing external impurities, vacuumizing and spraying gold on the surface.
The step 3 specifically comprises the following substeps:
(3a) the sample is immediately put into a drying oven at 105 +/-5 ℃ and dried to constant weight, then the sample is clamped by tweezers, floating particles on the surface of the sample are cleaned by an air gun, unnecessary pollution such as floating dust adhesion is avoided as much as possible, the observation section is guaranteed not to be disturbed, and the structure of the observation section is kept consistent with that of the original sample so as not to influence the observation result;
(3b) the sample and the sample plate are firmly bonded by the conductive adhesive, the position of a required interface is observed by attention, then the sample and the sample plate are placed in a gold plating device, the gold plating thickness is set to be 10nm, the top cover is closed, vacuum pumping is performed, gold spraying treatment is performed on the surface of the concrete sample, gold spraying lasts for 120 seconds each time, the uniformity of a gold spraying film is ensured, charge accumulation during imaging is avoided, white bright spots or interference fringes are generated, and real information is covered. The concrete metal spraying equipment adopts an SBC-12 small-sized ion sputtering instrument.
And 4, after the inspection is correct, the prepared sample is placed in a scanning electron microscope for observation, a typical interface of the sample is found under the low-magnification condition, and different interfaces are distinguished and numbered.
The method comprises the steps of irradiating a sample for 10 minutes in a short distance by using a desk lamp, observing the sample under a low-vacuum scanning electron microscope after a gold layer is solidified, adjusting and changing an observation area, comparatively investigating at least 3 areas of the same sample, firstly finding a typical interface of the sample under a low-magnification condition, then observing the sample under a gradual magnification, distinguishing two interfaces of a rubber coarse aggregate-cement paste interface (ITZ-X) and a regenerated coarse aggregate-cement paste interface (ITZ-Z), numbering the interfaces, and adopting a VGEA3 scanning electron microscope test system (Phenom Pro X Generation 5) of a Czech TESCAN company by using a scanning electron microscope.
And 5, selecting different magnification times to observe the samples, photographing different interfaces of each group of samples, and storing the pictures in a computer.
In order to facilitate the comparative analysis among different groups of test pieces, the magnification of the test pieces must be fixed and unified during observation, namely 4 magnifications are selected for each group of test pieces, namely four magnifications of 100 x, 2000 x, 5000 x and 10000 x are selected, 12 photos are taken on each interface, and 24 photos are taken in each sample and stored in a computer for research.
And 6, observing the appearances of a large number of interface transition areas, and finally selecting partial representative pictures to measure the width of the microcracks in the interface transition areas.
The step 6 specifically comprises the following substeps:
(6a) selecting SEM pictures with clear focus and resolution of at least 300 dpi/inch;
(6b) distinguishing areas where mortar, aggregate and an interface transition area appear;
the recycled rubber concrete is used as a composite material with multiphase composition, and obvious mutation exists in the gray value of an SEM image at the interface between different components. Firstly, calling an imhist command in MATLAB to obtain a gray level histogram of a scanned image of a concrete sample, and respectively extracting aggregate, mortar and an interface transition region in concrete by determining different threshold values. Wherein, the aggregate is darker and has a lower gray value, and the mortar is lighter and has a higher gray value.
(6c) The scale is marked in the picture, so that the size measurement of the microstructure is facilitated, and the low-power general survey and high-power observation means are facilitated;
(6d) the measurement function of SEM was used to determine the width of ITZ microcracks in the image;
(6d1) selecting the distance between the measuring points, wherein the length of the crack is l, and measuring every 1/3 l;
(6d2) clicking a mouse to select a point in the picture, setting the point as a starting point, clicking the mouse to select another point which is set as a terminal point, and displaying the distance between the two points on the picture, namely the width of the microcrack at the point, wherein the distance is shown in figure 3;
(6d3) the calculation formula of the width of the microcrack is shown in the formula (a);
wherein d isx(z)iDenotes the width of the micro-crack of this strip, d, ITZ-X (ITZ-Z)1/3lDenotes the width of the microcrack at 1/3l, d2/3lDenotes the width of the microcrack at 2/3l, dlThe width of the microcracks at l is indicated.
And 7, extracting the widths of the microcracks in the different interface transition regions, and calculating geometric parameters such as the average width, the maximum and minimum values, the standard deviation, the coefficient of variation and the like of the microcracks by adopting a statistical method to realize quantitative analysis of the widths of the microcracks in the interface transition regions.
(7a) The average width of the cracks is finally obtained by counting the crack width of each of two interface transition areas of an ITZ-X (ITZ-Z) image and then averaging the cracks with all widths, and the calculation formula can be expressed as follows:
wherein m represents the number of SEM image analyses per concrete sample, wherein i ═ 1, 2.. times, m,
represents the ITZ-X (ITZ-Z) mean microcrack width, and Σ represents the summing operation.
(7b) The maximum microcrack width was calculated according to equation (c):
dx(z),max＝max(dx(z)1,dx(z)2,dx(z)3......dx(z)m) (c)
wherein d isx(z),maxRepresents the ITZ-X (ITZ-Z) maximum microcrack width, and max () represents the max operation.
(7c) The minimum microcrack width is calculated according to equation (d):
dx(z),min＝min(dx(z)1,dx(z)2,dx(z)3......dx(z)m) (d)
wherein d isx(z),minRepresents the ITZ-X (ITZ-Z) minimum microcrack width, and min () represents the min operation.
(7d) Calculating the standard deviation according to equation (e):
wherein, σ represents a standard deviation,
indicating an open root operation.
(7e) The coefficient of variation is calculated as:
wherein, CVAnd the coefficient of variation is shown, and when the coefficient of variation is larger than 15 percent in the statistical analysis of the data, the data is considered to be abnormal and should be removed.
(7f) The detection results of the microcracks in the transition zone of the interface of the regenerated rubber concrete are shown in tables 2-3;
TABLE 2 ITZ-X statistical parameter table for microcrack width characteristic value
TABLE 3 ITZ-Z microcrack width eigenvalue statistical parameter table
Wherein, the maximum coefficient of variation is 9.50%, and the measurement result of the microcrack width has good convergence.
And 8, considering different interface transition areas, calculating the whole microcrack width of the test piece, and evaluating the mechanical property of the regenerated rubber concrete. The overall microcrack width calculation formula is shown in formula (g), and the compressive strength and overall microcrack width calculation results of the recycled rubber concrete of the embodiment are shown in table 4.
Wherein d represents the overall microcrack width, the rubber coarse aggregate content is α, and the recycled coarse aggregate content is β.
TABLE 4 compressive Strength of reclaimed rubber concrete and Overall Width calculation results
From FIG. 4, it can be observed that the compressive strength f is compared to the calculation of the overall microcrack widthcExhibit an opposite trend, d and fcHas good correlation, and the relation is as follows:
fc＝0.0445d3-0.3845d2-1.2664d+38.4963 (h)
research shows that the performance of the interface transition zone obviously affects the macroscopic mechanical property of the concrete, and the microscopic statistical result can approximately reflect the macroscopic mechanical property of the regenerated rubber concrete, such as compressive strength, to a certain extent. Therefore, for concrete buildings such as hydraulic engineering dams, nuclear power station engineering, military protective structures and the like which can not be drilled and sampled in large sizes, the microscopic structure analysis of small samples in the structure is carried out by using the electron microscope scanning technology, and the characterization of the macroscopic properties such as the structure quality and the like is feasible by using the microscopic indexes such as the microcrack width of the interface transition region and the like.
Claims (8)
1. A method for detecting the width of micro-cracks in a transition zone of a reclaimed rubber concrete interface is characterized by comprising the following steps:
step 1, preparing a regenerated rubber concrete test piece, and demolding after curing to a specified age;
step 2, cutting the regenerated rubber concrete test piece prepared in the step 1 into test pieces with the thickness not more than 15mm and the side length of 20mm multiplied by 20mm by a cutting machine to form at least four groups of test pieces;
step 3, placing the sample cut in the step 2 in a drying oven to be dried to constant weight, removing external impurities, vacuumizing and spraying gold on the surface;
4, placing the small sample subjected to gold spraying in the step 3 in a scanning electron microscope for observation, finding a typical interface of the sample under a low-magnification condition, distinguishing different interfaces and numbering;
step 5, selecting different magnification times to observe the samples, photographing different interfaces of each group of samples, and storing the pictures in a computer;
step 6, observing the appearance of the interface transition area, selecting a representative picture, and measuring the width of the microcracks in the interface transition area;
step 7, extracting the width of the microcracks in the transition regions of different interfaces, calculating the average width, the maximum and minimum values, the standard deviation and the variation coefficient of the microcracks, and realizing the quantitative analysis of the width of the microcracks in the transition regions of the interfaces;
and 8, calculating the whole microcrack width of the test piece, and evaluating the mechanical property of the regenerated rubber concrete.
2. The method for detecting the microcrack width of the transition zone of the recycled rubber concrete interface according to claim 1, wherein the section of the sample in the step 2 comprises an aggregate-cement slurry interface area, the surface of the section is relatively flat, and at least 3 samples are selected from each group of samples.
3. The method for detecting the microcrack width in the transition zone of the reclaimed rubber concrete interface according to claim 2, wherein the step 3 is specifically as follows:
step 3.1, placing the sample into a drying oven at 105 +/-5 ℃ for drying to constant weight, then clamping the sample by using tweezers, cleaning floating particles on the surface of the sample by using an air gun, and ensuring that the section is not disturbed when the sample is cleaned by using the air gun, so that the structure of the sample is consistent with that of the original sample;
and 3.2, firmly bonding the cleaned sample and the sample disc by using a conductive adhesive, then placing the sample disc into a gold plating device, setting the gold plating thickness to be 10nm, closing the top cover, vacuumizing, and carrying out gold spraying treatment on the surface of the sample, wherein the gold spraying lasts for 120 seconds each time until the set gold plating thickness is reached.
4. The method for detecting the microcrack width in the transition zone of the reclaimed rubber concrete interface according to claim 2, wherein the step 4 is specifically:
the method comprises the steps of irradiating a sample for 10 minutes at a short distance by using a table lamp, observing the sample under a low-vacuum scanning electron microscope after a gold layer is solidified according to a light source of 3-5cm, adjusting and changing an observation area, observing at least 3 areas by using one sample, wherein each area comprises two interfaces of a rubber coarse aggregate-cement paste interface and a regenerated coarse aggregate-cement paste interface, finding a typical interface of the sample under a low-magnification condition, observing the typical interface by gradually magnifying the typical interface by multiple, distinguishing the two interfaces of the rubber coarse aggregate-cement paste interface and the regenerated coarse aggregate-cement paste interface, and numbering the two interfaces.
5. The method for detecting the microcrack width in the transition zone of the reclaimed rubber concrete interface according to claim 4, wherein the step 5 is specifically as follows:
each sample group is selected from 4 magnifications, namely four magnifications of 100 x, 2000 x, 5000 x and 10000 x are selected, 4 magnifications are taken for each interface, at least 24 photos are taken for one sample group, at least three samples are taken for each sample group, at least 24 x 3 pictures are taken for one sample group, 72 photos are taken for one sample group, and at least 72 x 4 pictures are taken for four sample groups, and the photos are stored in a computer.
6. The method for detecting the microcrack width in the transition zone of the reclaimed rubber concrete interface according to claim 1, wherein the step 6 specifically comprises:
6.1, selecting an SEM picture which is clear in focus and has the resolution of at least 300 dpi/inch;
6.2, distinguishing areas of mortar, aggregate and interface transition areas in the picture;
step 6.3, scaling in the picture;
step 6.4, determining the width of the ITZ microcracks in the image by using the measurement function of the SEM;
6.5, selecting the measuring point space, wherein the crack length is l, and measuring every 1/3 l;
6.6, clicking a mouse to select a point in the picture, setting the point as a starting point, clicking the mouse to select another point, setting the point as a terminal point, and displaying the distance between the two points on the picture, namely the width of the microcrack at the point;
step 6.7, calculating the width of the microcrack: calculating a formula shown in formula (a);
wherein d isx(z)iIndicates the width of the micro-crack in the rubber coarse aggregate-cement paste interface or the recycled coarse aggregate-cement paste interface, wherein when d isx(z)iSubscript x, i.e. dxiShowing the microcrack width at the rubber coarse aggregate-cement slurry interface in the ith image when dx(z)iThe subscript being z, i.e. dziDenotes the microcrack width at the recycled coarse aggregate-cement slurry interface in the ith image, d1/3lDenotes the width of the microcrack at 1/3l, d2/3lDenotes the width of the microcrack at 2/3l, dlThe width of the microcracks at l is indicated.
7. The method for detecting the microcrack width in the transition zone of the reclaimed rubber concrete interface according to claim 6, wherein the step 7 is specifically as follows:
step 7.1, calculating the width of each crack in the transition area of each sample rubber coarse aggregate-cement paste interface and the regenerated coarse aggregate-cement paste interface respectively according to the step 6, averaging the cracks with all widths, and finally obtaining the average width of the cracks, wherein the calculation formula can be expressed as follows:
wherein m represents the number of SEM image analyses per sample, dx(z)iThe average microcrack width at the rubber coarse aggregate-cement slurry interface or recycled coarse aggregate-cement slurry interface in the ith image is shown, where i is 1, 2.. multidot.m,
the average microcrack width of the rubber coarse aggregate-cement paste interface or the regenerated coarse aggregate-cement paste interface is shown, and sigma represents summation operation;
step 7.2, respectively calculating the maximum microcrack width of the interface of the medium rubber coarse aggregate-cement paste or the interface of the regenerated coarse aggregate-cement paste:
dx(z),max＝max(dx(z)1,dx(z)2,dx(z)3......dx(z)m) (c)
wherein d isx(z),maxRepresents the maximum microcrack width in the rubber coarse aggregate-cement paste interface or the regenerated coarse aggregate-cement paste interface, and max () represents the operation of solving the maximum value;
step 7.3, respectively calculating the minimum microcrack width of the interface of the medium rubber coarse aggregate-cement paste or the interface of the regenerated coarse aggregate-cement paste:
dx(z),min＝min(dx(z)1,dx(z)2,dx(z)3......dx(z)m) (d)
wherein d isx(z),minRepresenting the minimum microcrack width in the rubber coarse aggregate-cement paste interface or the regenerated coarse aggregate-cement paste interface, and min () representing the minimum value solving operation;
step 7.4, respectively calculating the standard deviation of the interface of the medium rubber coarse aggregate-cement paste or the interface of the recycled coarse aggregate-cement paste:
wherein, σ represents a standard deviation,
representing root number opening operation;
step 7.5, respectively calculating the variation coefficient of the medium rubber coarse aggregate-cement paste interface or the regenerated coarse aggregate-cement paste interface:
wherein, CVRepresenting the coefficient of variation, and eliminating the data if the coefficient of variation is more than 15% during data statistical analysis.
8. The method for detecting the microcrack width of the transition zone of the reclaimed rubber concrete interface according to claim 7, wherein the step 8 of calculating the microcrack width of the whole test piece specifically comprises the following steps:
wherein d represents the width of the whole microcracks, the content of the rubber coarse aggregate is α, the content of the recycled coarse aggregate is β, and d represents the total microcracksxiDenotes the microcrack width at the rubber coarse aggregate-cement slurry interface in the ith image, dziShowing the microcrack width at the recycled coarse aggregate-cement slurry interface in the ith image.
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