CN116735448A - Method for characterizing porosity of interface transition zone in concrete based on image analysis - Google Patents
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Abstract
The invention discloses an image analysis-based characterization method for the porosity of an interface transition zone in concrete. The method comprises the following steps: 1) Acquiring a back scattering electron microscope image containing an interface transition region in concrete; 2) Carrying out gray scale treatment on the image and calibrating the size; 3) Determining an interface transition region of the back image, marking the boundary of the interface transition region, and carrying out equidistant strip division on the interface transition region to obtain a plurality of subdivision bands; 4) Dividing the aperture of each sub-band by a threshold method, determining an optimal threshold value, and determining the total area of each sub-band and the area of the hole according to the gray level; 5) The porosity of each zonal segment was calculated and a porosity curve was drawn for the interfacial transition zone to aggregate/fiber distance. The method is based on the difference of gray scales of the internal composition of the concrete, such as pores, a matrix, aggregate/fiber and the like, accurately identifies the boundary of the components, quantitatively characterizes the porosity of the interface transition region finally and confirms the thickness of the interface transition region, and is simple and easy to operate and high in analysis precision.
Description
Technical Field
The invention relates to the technical field of computer image analysis of building materials, in particular to an image analysis-based method for characterizing the porosity of an interface transition zone in concrete.
Background
Concrete is a typical multiphase, multi-scale structure formed by setting and hardening after mixing cement, aggregate, water, additives and the like, and generally comprises four scales of macroscopic, microscopic and nanoscopic. The concrete is mainly composed of aggregate, a matrix and an aggregate-matrix interface transition zone under the microscopic scale, and can be researched by adopting an electron microscope and an optical microscope, wherein the interface transition zone between aggregate and cement paste under the hierarchy is a remarkable characteristic of the concrete structure. During the concrete formulation process, a water film is formed around large particle aggregates or rebars, etc., which results in a higher water cement ratio around them than the matrix itself. Meanwhile, calcium, sulfate radical and aluminate ions generated by dissolution of cement clinker, gypsum and the like can be combined with cement paste to generate ettringite and calcium hydroxide firstly. Because of the high water to ash ratio around the aggregate, the crystallized product is coarse and porous, and therefore, a transition structure with more pores than the cement slurry or mortar body can be formed. The thickness of the fiber, aggregate and cement-based interfacial layer is typically 50-100 μm, with hardness varying primarily with matrix characteristics. The original crack increases and becomes larger in the interface area, and is a weak area which is damaged firstly after being stressed. The fiber-matrix interface layer has the characteristics of higher water-cement ratio and porosity than the matrix, loose network structure than the matrix, and the like, CH crystals in the interface layer are arranged in an oriented manner, the orientation index is high, the orientation range is large, and the content of the CH crystals is generally 20% -40% higher than that of the matrix.
Since plain concrete has typical brittleness, reinforcing materials such as steel bars or steel fibers are generally incorporated into the inside of the concrete in order to improve its tensile strength and toughness. The reinforcing material is added to increase the interface transition area between the reinforcing steel bar and the matrix and between the fiber and the matrix, and the quality of the interface transition area directly influences the bonding performance of the reinforcing steel bar and the fiber and the matrix, the mechanical performance of the final fiber reinforced concrete, and the like. The quality of the interface transition zone in the concrete can be usually characterized by adopting a microhardness method, a nanoindentation method and the like. Microhardness and nanoindentation methods can quantitatively characterize the micromechanics of the interfacial transition, but they generally require that the test piece be very flat and require a large amount of statistical data, while it is difficult to quantitatively describe the thickness and porosity of the interfacial transition. BSEM analysis is a popular means widely used for characterization of building material properties, and can be used for analyzing chemical components of micro-areas in cement-based materials, distinguishing different phases and microstructures, quantifying the volume content of a statistical phase, researching hydration degree, and qualitatively and quantitatively analyzing pore structures. The gray level of BSEM depends on the average atomic number of different micro-region phases, and the higher the average atomic number of the sample surface is, the stronger the generated back scattering electronic signal is, the higher the brightness of the image in BSEM is, and the smaller the gray level is. In portland cement hardened slurries, the gray scale values of BSEM images can be roughly divided from dark to light: pore or crack, hydrated calcium silicate gel, calcium Hydroxide (CH) and unhydrated cement clinker.
At present, the related literature of the porosity characterization method of the interface transition zone in concrete is not published until now. Although CN113155042B discloses a method for measuring the thickness of an interface transition zone in concrete, the method adopts an image observation method to obtain a compressive deformation image of a concrete test block, processes and analyzes displacement deformation conditions of each zone in the image, and finally calculates the thickness of the interface transition zone, the method does not involve calculation and characterization of porosity of the interface transition zone; CN110458816a discloses a method of analysis of porosity of a fibrous material based on threshold regression, however the internal microstructure of a multi-scale concrete material is far more complex than that of a fibrous material. In view of the complexity and randomness of the interfacial transition region in concrete, a brand new characterization method of the porosity of the interfacial transition region in concrete needs to be explored.
Disclosure of Invention
The invention aims to provide an image analysis-based method for characterizing the porosity of an interface transition zone in concrete. The method utilizes the prior image technology to accurately identify the boundary of the components based on the difference of gray scales of the internal composition of the concrete such as pores, matrixes, aggregates/fibers and the like, and finally quantitatively characterizes the porosity of the interface transition region and confirms the thickness of the interface transition region, and the method is simple and easy to operate and has high analysis precision.
The technical scheme of the invention is as follows: an image analysis-based characterization method for the porosity of an interface transition zone in concrete comprises the following steps:
1) Acquiring a back scattering electron microscope image containing an interface transition region in concrete;
2) Gray scale processing is carried out on the back scattering electron microscope image, and the size is calibrated;
3) Determining an interface transition region of the back scattering electron microscope image, marking the boundary of the interface transition region, and carrying out equidistant strip division on the interface transition region to obtain a plurality of subdivision bands;
4) Dividing the aperture of each sub-band by a threshold method, determining an optimal threshold value, and determining the total area of each sub-band and the area of the hole according to the gray level;
5) The porosity of each zonal segment was calculated and a porosity curve was drawn for the interfacial transition zone to aggregate/fiber distance.
In the step 1) of the method for characterizing the porosity of the transition zone of the concrete interface based on image analysis, the concrete is a near-cube sample with the size of 1-2 cm. The sampling structure is beneficial to observing the material composition and structure in the concrete.
In the step 1) of the method for characterizing the porosity of the transition zone of the concrete interface based on image analysis, the concrete needs to be pretreated as follows: soaking in absolute alcohol for 1d, and drying at 60+ -2deg.C for 48 hr. By this treatment, hydration can be terminated, and because of the presence of free water in the concrete, cement reacts with water to form other hydration products, resulting in changes in the content and structure of the pore structure, unhydrated cement, etc., and the presence of water affects the quality of SEM image observation by electron microscopy.
In the method for characterizing the porosity of the transition zone of the concrete interface based on image analysis, the pretreated concrete is stored in a sealed dry environment.
In the step 1) of the method for characterizing the porosity of the transition zone of the concrete interface based on image analysis, the concrete needs to be pretreated as follows: the concrete surface is firstly subjected to rough grinding, then is impregnated with resin, is finely ground, and finally is polished by adopting suspension liquid and is cleaned by adopting ultrasonic waves. BSEM testing requires that the surface of the sample be very flat and smooth, based on which the sample surface is to be sanded and polished. The resin-impregnated sample mainly plays a role of protecting and supporting the microstructure, because steel fibers, aggregates and cement paste are arranged in the concrete, and the fibers and the aggregates are harder than the cement paste so as not to damage the internal microstructure.
In the step 1) of the method for characterizing the porosity of the concrete interface transition zone based on image analysis, the interface transition zone is an interface transition zone of aggregate-matrix or an interface transition zone of fiber/reinforcement-matrix; the water-gel ratio of the matrix is 0.18-0.6.
In the step 3) of the method for characterizing the porosity of the concrete interface transition region based on image analysis, when the interface transition region is divided into equidistant strips, 5-10 subdivision strips are determined according to the marked boundary shape and the concentric expansion method, and each subdivision strip has a bandwidth of 5-10 mu m. The inventors have found through extensive experimental summary analysis that the internal interface transition zone of concrete is typically about 30-100 μm thick. Furthermore, if the stripe width is too small, the resolution of the picture is low, which is difficult to divide, and if it is too thick, the accuracy of measurement is lowered. Therefore, the inventor finally determines the optimal range of the width of the strip according to the total range and by comprehensively analyzing and considering the measurement precision and the resolution.
In the step 4) of the method for characterizing the porosity of the transition zone of the concrete interface based on image analysis, the optimal threshold is determined by adopting a tangential intersection method.
In the step 5) of the concrete interface transition area porosity quantitative characterization method based on image analysis, the porosity of each zonal is equal to the internal pore area divided by the total area of the zonal.
The beneficial effects are that: compared with the prior art, the invention provides the method for characterizing the porosity of the interface transition zone in the concrete based on image analysis, which can effectively characterize the porosity of the interface transition zone in the concrete, including the fiber-matrix interface transition zone, the aggregate-matrix interface transition zone and the like, according to the acquired BSEM image and by means of image processing software. At present, no report of quantitatively analyzing the porosity of an interface transition region in concrete by an image recognition method exists, the BSEM image of the interface transition region is shot, the interface transition region in the concrete is divided into strips with the width of 5-10 mu m by a concentric expansion method by using a computer image processing technology, the porosity of each strip is divided by a threshold method, and the porosity of each strip is obtained by calculation. The porosity analysis of the interface transition zone is provided for the first time, not only can accurately represent the microstructure inside the concrete, but also can provide theoretical basis and reference for the performance macroscopic performance development, performance degradation, reinforcement mechanism analysis and discussion and the like of the concrete.
In summary, the invention utilizes advanced image processing technology to accurately identify the boundary of components based on the difference of gray scales of the internal composition of concrete such as pores, matrix, aggregate/fiber and the like, and finally quantitatively characterize the porosity and thickness of the interface transition region, and has the advantages of visual and clear image, low cost, simplicity, easy operation and high efficiency.
Drawings
FIG. 1 is a BSEM of an interfacial transition zone division strip in a concrete sample of an embodiment of the present invention;
FIG. 2 is a segmentation of a first strip of an interfacial transition zone in a concrete sample according to an embodiment of the present invention;
FIG. 3 is a graph of gray scale segmentation of voids from an image of an interfacial transition zone in a concrete sample of the present invention;
FIG. 4 is a graph of porosity as a function of thickness in the interfacial transition zone of a concrete sample of the present invention.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to be limiting.
The principle basis is as follows:
the method for characterizing the porosity of the interface transition zone in the concrete is based on a gray image processing technology, and the concrete mainly comprises aggregate, fiber or steel bar, a cement matrix, an aggregate-matrix interface transition zone and/or a fiber-matrix interface transition zone, a pore structure and the like in composition, wherein the gray and the size of different materials are obviously different. In view of the fact that the porosity of the interface transition area in the concrete is obviously higher than that of the matrix, by means of an image analysis method, the boundary of the interface is determined, then concentric circular strips are drawn around the fiber or the aggregate at intervals by a concentric expansion method, the pore of each strip is divided by a threshold method, the total area of each strip and the area of the hole are calculated through gray processing, the porosity of each strip is finally calculated, the change rule of the porosity along with the distance from the aggregate/fiber boundary is further drawn, the porosity of the interface transition area is finally quantized, and the thickness of the interface transition area can be determined. The inventor researches find that the interface transition zone is usually in the intermediate zone between the aggregate or the fiber and the cement paste. Therefore, aiming at the irregular aggregate or fiber appearance, the aggregate or fiber appearance is drawn into a concentric circle strip at intervals outwards, the actual situation of the porosity can be reflected more accurately, and the porosity obtained by final calculation is more accurate.
Example 1. The method for characterizing the porosity of the interface transition zone in the concrete based on image analysis comprises the steps of obtaining a concrete polishing test block containing the interface transition zone; obtaining a back scattering image of the interface transition region by utilizing an electronic scanning technology; performing gray scale processing on the back scattering image by using image analysis software; identifying and calibrating the boundary of the interface area and dividing the boundary into a plurality of equal distances according to a concentric expansion method; dividing the pores of each interface transition zone by adopting a threshold method and determining an optimal threshold; determining the total area of each small interface transition zone (subdivision zone) and the area of the hole by using an image analysis and calculation function; and calculating the porosity and drawing a porosity curve for drawing the distance between the interface transition region and the aggregate/fiber.
Specifically, cement-based materials are selected as a test piece matrix, a steel fiber is embedded in the matrix, the length of the steel fiber is 13mm, the diameter of the steel fiber is 0.2mm, casting is completed for 24 hours, demolding is completed, and standard curing is carried out until 28d; after curing for 28d, cutting a sample of the strip steel fiber from the test piece, wherein the length and the width are about 2cm, immediately soaking the cut sample in absolute alcohol for 1d, drying at the temperature of (60+/-2) ℃ for 48h, and sealing, drying and preserving for later use;
the surface of the sample is firstly subjected to rough polishing, then is impregnated with resin, is finely polished by polishing papers with different roughnesses, is finally polished by suspension, is subjected to ultrasonic cleaning for 5 minutes, and is stored in a sealed and dry environment. And (3) putting the prepared samples into a spraying instrument for carbon spraying or metal spraying, then using a Hetachi S4700-SEM scanning electron microscope to detect each sample under a Back Scattering Electron (BSEM) mode by using an accelerating voltage of 15kV, and obtaining BSEM images to be analyzed through amplification of 200 times and 250 times. And converting the acquired BSEM image containing the interface transition region into an 8-bit gray scale image by using imageJ image analysis software, and calibrating the image size.
The boundaries of fibers in the processed images are identified and marked by adopting a linear mode, then an interface transition zone strip is marked outwards at intervals of 10um by a concentric expansion method according to the marked boundary lines (figure 1), and the marked strip images are sequentially segmented, as shown in figure 2.
Dividing the aperture of the extracted interface transition zone band image by a threshold method, and determining an optimal threshold by a tangential intersection method; the threshold is an important parameter for calculating porosity in the gray scale map, and different thresholds can result in a change in the area of the separated pores. The tangent intersection point method is to obtain the curve of gray value (X axis) and area dividing ratio (Y axis) by image software, and then draw tangent to two ascending sections of the curve, the intersection point is the optimal threshold. And meanwhile, the band segmentation image (figure 3) after gray level processing is obtained by adjusting gray level, and the hole area of each small interface transition area and the total area of the band are directly obtained by the analysis and calculation function of software.
The resulting void area within each interfacial transition zone divided by the total pore area is the porosity of each strip.
And drawing according to the obtained porosity of each strip and the distance from the boundary to obtain the change rule of the porosity along with the distance of the interface transition region, as shown in fig. 4.
The invention quantifies the porosity of the interface transition zone in the concrete by using an image processing technology based on the gray level difference in the BSEM of each component material in the concrete; the method has simple and clear implementation steps and extremely high operability.
And the invention is not limited to the above embodiments, but any obvious modifications, substitutions, etc. can be made by one skilled in the art without departing from the spirit of the invention.
Claims (9)
1. The method for characterizing the porosity of the interface transition zone in the concrete based on image analysis is characterized by comprising the following steps of: the method comprises the following steps:
1) Acquiring a back scattering electron microscope image containing an interface transition region in concrete;
2) Gray scale processing is carried out on the back scattering electron microscope image, and the size is calibrated;
3) Determining an interface transition region of the back scattering electron microscope image, marking the boundary of the interface transition region, and carrying out equidistant strip division on the interface transition region to obtain a plurality of subdivision bands;
4) Dividing the aperture of each sub-band by a threshold method, determining an optimal threshold value, and determining the total area of each sub-band and the area of the hole according to the gray level;
5) The porosity of each zonal segment was calculated and a porosity curve was drawn for the interfacial transition zone to aggregate/fiber distance.
2. The method for characterizing the porosity of the transition zone of the concrete interface based on image analysis according to claim 1, wherein: in step 1), the concrete is a near-cubic sample of 1 to 2 cm.
3. The method for characterizing the porosity of an interface transition zone in concrete based on image analysis according to claim 1, wherein: in step 1), the concrete needs to be pretreated as follows: soaking in absolute alcohol for 1d, and drying at 60+ -2deg.C for 48h.
4. The method for characterizing interfacial transition zone porosity in concrete based on image analysis according to claim 3, wherein: the pretreated concrete is preserved in a sealed dry environment.
5. The method for characterizing the porosity of an interface transition zone in concrete based on image analysis according to claim 1, wherein: in step 1), the concrete needs to be pretreated as follows: the concrete surface is firstly subjected to rough grinding, then is impregnated with resin, is finely ground, and finally is polished by adopting suspension liquid and is cleaned by adopting ultrasonic waves.
6. The method for characterizing the porosity of an interface transition zone in concrete based on image analysis according to claim 1, wherein: in the step 1), the interface transition zone is an interface transition zone of an aggregate-matrix or an interface transition zone of a fiber/reinforcement-matrix; the water-gel ratio of the matrix is 0.18-0.6.
7. The method for characterizing the porosity of an interface transition zone in concrete based on image analysis according to claim 1, wherein: in the step 3), when the interface transition zone is divided into equidistant strips, 5-10 subdivision strips are determined according to the marked boundary shape and the concentric expansion method, and each subdivision strip has a bandwidth of 5-10 mu m.
8. The method for characterizing the porosity of an interface transition zone in concrete based on image analysis according to claim 1, wherein: in step 4), the optimal threshold is determined by a tangential intersection method.
9. The method for characterizing the porosity of an interface transition zone in concrete based on image analysis according to claim 1, wherein: in step 5), the porosity of each of the bands is equal to the internal pore area divided by the total area of the bands.
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| CN117805156B (en) * | 2024-02-27 | 2024-05-10 | 太原理工大学 | Method for testing hydration degree of interface transition zone between repair material and base material |
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