CN111610213A - Quantitative analysis method for microstructure of rubber concrete - Google Patents

Quantitative analysis method for microstructure of rubber concrete Download PDF

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CN111610213A
CN111610213A CN202010651919.2A CN202010651919A CN111610213A CN 111610213 A CN111610213 A CN 111610213A CN 202010651919 A CN202010651919 A CN 202010651919A CN 111610213 A CN111610213 A CN 111610213A
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concrete
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rubber concrete
rubber
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CN111610213B (en
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王娟
邓宇
张鹏
管俊峰
许耀群
葛巍
郭祯祥
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Zhengzhou University
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    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract

The invention discloses a quantitative analysis method for a microstructure of rubber concrete, which comprises the following steps: preparing a rubber concrete sample, treating the rubber concrete sample, observing the microstructure appearance of a sample cutting block, measuring the pore structure of the sample cutting block and analyzing the relation between the microstructure and the macroscopic strength; the invention firstly observes the microstructure of a sample cut block through a scanning electron microscope system, then measures the pore structure on the sample cut block through a linear wire method, and then tests the compressive strength of the rubber concrete through a hydraulic servo universal testing machine, thereby obtaining the influence of the microstructure of the rubber concrete on the macroscopic strength through the analysis of the microstructure test and the macroscopic mechanical property test, and further providing great help for the performance prediction and improvement of the rubber concrete in the aspects of water conservancy, civil engineering, traffic and the like.

Description

Quantitative analysis method for microstructure of rubber concrete
Technical Field
The invention relates to the technical field of material performance analysis, in particular to a quantitative analysis method for a microstructure of rubber concrete.
Background
The rubber concrete is prepared by mixing, molding and curing rubber emulsion, auxiliary additives and cement when cement mortar or concrete is prepared, has excellent impact resistance and wear resistance, and can better solve the problem of recycling waste rubber products at the same time;
in order to promote the popularization and application of rubber concrete in actual engineering such as water conservancy, civil engineering, traffic and the like, the structural strength and the fracture performance of the rubber concrete need to be analyzed to reveal the strength reduction mechanism of the rubber concrete and prolong the service life of a concrete structure.
Disclosure of Invention
Aiming at the problems, the invention aims to provide a quantitative analysis method for a microstructure of rubber concrete, which adopts a scanning electron microscope and a hardened concrete pore structure parameter analyzer to respectively observe microstructures such as hydration products, microcracks, microporosities and the like in the rubber concrete at different ages, and analyzes the influence of the microstructure of part of the rubber concrete on the macroscopic strength by comparing the compressive strength test result.
In order to achieve the purpose of the invention, the invention is realized by the following technical scheme: a quantitative analysis method for a microstructure of rubber concrete comprises the following steps:
the method comprises the following steps: preparation of rubber concrete samples
Cleaning a stirrer and coating slurry on the inner wall of the stirrer, sequentially adding weighed coarse aggregate, fine aggregate, rubber particles, cement and sand into the stirrer and stirring for 2 minutes, adding weighed water into the stirrer and continuously stirring for 2 minutes, unloading concrete onto a steel plate after uniform stirring and immediately carving the concrete into a test mold, then placing the test mold on a vibration table and vibrating for 1 minute, plastering the upper surface of the concrete after the concrete is formed, covering the test mold with wet cloth and standing the test mold indoors for 24 hours, and finally demolding the rubber concrete and placing the rubber concrete into a standard curing room for curing to obtain a rubber concrete sample;
step two: rubber concrete sample treatment
According to the first step, a rubber concrete sample is maintained in a standard curing room to different specified ages, after the maintenance time reaches the standard, a cutting machine is used for cutting the sample into sample blocks with the length and width of 10 x 10mm for scanning by an electron microscope and sample slices with the length and width of 100 x 15mm for analyzing a hole structure, then the sample blocks are placed in a drying oven for heating and drying treatment, the heating temperature is set to be 50 ℃, after drying, gold spraying is carried out on the observation surface of the sample blocks, then the observation surface of the sample slices is blackened, after blacking, the sample slices are placed in the drying oven for drying, after drying, a layer of white barium sulfate powder is scattered on the blackened observation surface, and the white barium sulfate powder is moved and pressed to fill the holes in the observation surface of the whole sample slices;
step three: observing the microstructure morphology of the sample cut
According to the second step, firstly, opening a scanning electron microscope system and operating control software to enable the vacuum degree of the sample chamber to return to the atmosphere, then loading the prepared sample blocks into the sample chamber and evacuating the sample chamber, then setting the parameter values of voltage, current and definition, observing the appearance of hydration products on the observation surface of the sample blocks through adjusting the multiplying power and a teaching aid, then marking the length, width and position information of microcracks on the observation surface of the sample blocks, and storing and exporting marked pictures;
step four: measurement sample section pore structure
According to the second step, measuring the geometric parameters of the pores in the observation surface of the rubber concrete sample slice by adopting a straight line wire method, firstly setting a region with the surface middle position of the observation surface of the sample slice being 50 multiplied by 50mm as an observation region, then dividing the observation region into 63 subregions with the same size and sequentially collecting the images of each subregion, wherein the number of the subregions with the same size is changed along with the area change of the total observation region, then determining a threshold value and converting the collected images into binary images so as to improve the identification effect of the pores, then measuring the number and the chord length of the pores of each subregion by adopting the straight line wire method, calculating the total number and the chord length of the pores of the whole observation region, and finally calculating the statistical value of the geometric parameters of the pores of the whole;
step five: analyzing the relationship between microstructure and macroscopic strength
According to the fourth step, firstly, a hydraulic servo universal testing machine is adopted to carry out a compressive strength test on the rubber concrete, the compressive strengths of the rubber concrete at different curing ages are compared, and then the relation between the microstructure and the macroscopic strength of the rubber concrete is obtained through analysis according to the microstructure observation result of the rubber concrete sample block and the measurement result of the rubber concrete sample block pore mechanism and by combining the compressive strength comparison results of the rubber concrete at different curing ages.
The further improvement lies in that: in the first step, the ratio of water to cement to sand to fine aggregate to coarse aggregate to rubber particles is 2:4:5:3:8:1, the uniformly stirred concrete is cleaned by wiping the test mold before being added into the test mold, a layer of release agent is uniformly coated on the concrete, and the test mold is vibrated under pressure when vibrated on a vibration table so as to prevent the rubber particles from floating upwards.
The further improvement lies in that: and in the second step, before the sample slice is blackened and dried, an automatic polishing machine is adopted to polish the observation surface of the sample slice, a coarse-to-fine abrasive is used for polishing in the polishing process, after polishing is finished, the residue on the surface of the sample slice is washed away by flowing clear water, and then the sample slice is put into an ultrasonic cleaning instrument for cleaning.
The further improvement lies in that: and in the second step, spraying gold on the observation surface of the sample slice by a gold spraying instrument, keeping the current at 8mA during spraying gold, setting the gold spraying time to be 3 minutes, and repeatedly blacking the observation surface of the sample slice horizontally and vertically in sequence by a black water-based pen.
The further improvement lies in that: in the fourth step, 63 sub-regions with the same size are composed of 7 sub-regions in the horizontal direction and 9 sub-regions in the vertical direction.
The further improvement lies in that: in the fourth step, the calculation formula is
Figure BDA0002575295790000041
Figure BDA0002575295790000042
Figure BDA0002575295790000043
Figure BDA0002575295790000044
Wherein A is porosity, ∑ l is the sum of chord lengths of bubbles cut by the whole wire, and T is the wireThe total length of the device is as long as,
Figure BDA0002575295790000045
is the average chord length of the bubbles, n is the total number of the bubbles cut by the whole wire, r is the average radius of the bubbles,
Figure BDA0002575295790000051
is the bubble spacing coefficient, p is the slurry content in the concrete, n1The number of air bubbles cut per 10mm wire on average.
The invention has the beneficial effects that: the invention firstly prepares a representative rubber concrete test sample through reasonable raw material proportion, then cuts, dries and metal spraying the sample according to the observation test requirement of a scanning electron microscope to obtain a sample cut block for scanning the electron microscope, then cuts, dries, blackens and sprays barium sulfate powder to the sample according to the analysis test requirement of the pore structure to obtain a sample slice for analyzing the pore structure, then observes the microstructure of the sample cut block through a scanning electron microscope system, measures the pore structure on the sample slice through a linear wire method, and then carries out a compressive strength test on the rubber concrete through a hydraulic servo universal testing machine, thereby obtaining the influence of the microstructure of the rubber concrete on the macroscopic strength through the analysis of the microstructure test and the macroscopic mechanical property test, and further providing great help for the performance prediction and improvement of the rubber concrete in the aspects of water conservancy, civil engineering, traffic and the like, the analysis method is scientific and rigorous, is practical, and has representative conclusion obtained by analysis.
Drawings
FIG. 1 is a flow chart of the steps of the present invention;
FIG. 2 is a flow chart of the preparation of rubber concrete samples according to the present invention.
Detailed Description
In order to further understand the present invention, the following detailed description will be made with reference to the following examples, which are only used for explaining the present invention and are not to be construed as limiting the scope of the present invention.
According to fig. 1 and 2, the present embodiment provides a method for quantitatively analyzing a microstructure of rubber concrete, comprising the following steps:
the method comprises the following steps: preparation of rubber concrete samples
Cleaning a test mould, uniformly coating a layer of release agent, cleaning a stirrer, allowing the inner wall of the stirrer to be coated with slurry, sequentially adding weighed coarse aggregate, fine aggregate, rubber particles, cement and sand into the stirrer, stirring for 2 minutes, adding weighed water into the stirrer, continuously stirring for 2 minutes, wherein the mixing ratio of the water, the cement, the sand, the fine aggregate, the coarse aggregate and the rubber particles is 2:4:5:3:8:1, unloading the concrete onto a steel plate after uniform stirring, vertically carving, filling the concrete into the test mould, placing the test mould on a vibrating table, pressurizing and vibrating for 1 minute, coating the upper surface of the concrete after the concrete is formed, covering the test mould with wet cloth, standing for 24 hours indoors, demolding the rubber concrete, and placing the rubber concrete into a standard curing chamber for curing to obtain a rubber concrete sample;
step two: rubber concrete sample treatment
According to the first step, the rubber concrete sample is maintained in a standard curing room to different specified ages, after the maintenance time reaches the standard, the sample is cut into sample blocks with the length and width of 10 multiplied by 10mm for scanning by an electron microscope and sample slices with the length and width of 100 multiplied by 15mm for analyzing the hole structure by a cutting machine, then the sample blocks are put into an oven for heating and drying treatment, the heating temperature is set to be 50 ℃, after drying, the observation surfaces of the sample blocks are sprayed with gold by a gold spraying instrument, the current is kept at 8mA during gold spraying, the gold spraying time is set to be 3 minutes, then an automatic polishing machine is adopted to polish the observation surfaces of the sample blocks, the polishing process is carried out by using a coarse and fine abrasive material, after polishing, surface residues are washed off by flowing clear water, then the sample blocks are put into an ultrasonic cleaning instrument for cleaning, then the observation surfaces of the sample blocks are sequentially and vertically repeatedly blackened by a black water pen, then, a layer of white barium sulfate powder is scattered on the blackened observation surface and moved and pressed to fill the pores on the observation surface of the whole sample slice;
step three: observing the microstructure morphology of the sample cut
According to the second step, firstly, opening a scanning electron microscope system and operating control software to enable the vacuum degree of the sample chamber to return to the atmosphere, loading the prepared sample blocks into the sample chamber and evacuating the sample chamber, then setting the parameter values of voltage, current and definition, observing the appearance of hydration products on the observation surface of the sample blocks through adjusting the multiplying power and a teaching aid, then marking the length, width and position information of microcracks on the observation surface of the sample blocks, and storing and exporting marked pictures;
step four: measurement sample section pore structure
According to the second step, the geometric parameters of the pores in the observation surface of the rubber concrete sample are measured by adopting a straight line wire method, a region with the middle position of 50 x 50mm on the surface of the observation surface of the sample slice is firstly set as an observation region, the observation region is divided into 63 subregions with the same size, images of each subregion are sequentially collected, wherein the 63 subregions with the same size consist of 7 subregions in the horizontal direction and 9 subregions in the vertical direction, the number of the subregions with the same size is changed along with the area change of the total observation region, then a threshold value is determined, the collected images are converted into binary images to improve the identification effect of the pores, then the number and the chord length of the pores of each subregion are measured by adopting a straight line wire method, the total number and the chord length of the pores of the whole observation region are calculated, and finally the, the formula is
Figure BDA0002575295790000071
Figure BDA0002575295790000072
Figure BDA0002575295790000073
Figure BDA0002575295790000074
Wherein A is porosity, ∑ l is the sum of chord lengths of bubbles cut by the whole wire, T is the total length of the wire,
Figure BDA0002575295790000081
is the average chord length of the bubbles, n is the total number of the bubbles cut by the whole wire, r is the average radius of the bubbles,
Figure BDA0002575295790000082
is the bubble spacing coefficient, p is the slurry content in the concrete, n1The number of air bubbles cut per 10mm of wire on average;
step five: analyzing the relationship between microstructure and macroscopic strength
According to the fourth step, firstly, a hydraulic servo universal testing machine is adopted to carry out a compressive strength test on the rubber concrete, the compressive strengths of the rubber concrete at different curing ages are compared, and then the relation between the microstructure and the macroscopic strength of the rubber concrete is obtained through analysis according to the microstructure observation result of the rubber concrete sample block and the measurement result of the rubber concrete sample block pore mechanism and by combining the compressive strength comparison results of the rubber concrete at different curing ages.
The quantitative analysis method of the microstructure of the rubber concrete comprises the steps of preparing a representative rubber concrete test sample according to a reasonable raw material ratio, cutting, drying and metal spraying the sample according to the observation test requirement of a scanning electron microscope to obtain a sample cutting block for scanning of the electron microscope, cutting, drying, blackening and scattering barium sulfate powder on the sample according to the analysis test requirement of the pore structure to obtain a sample slice for analyzing the pore structure, observing the microstructure of the sample cutting block through a scanning electron microscope system, measuring the pore structure on the sample cutting block through a linear wire method, and carrying out a compressive strength test on the rubber concrete through a hydraulic universal servo testing machine, so that the influence of the microstructure of the rubber concrete on the macroscopic strength is analyzed through a microstructure test and a macroscopic mechanical property test, and further the influence of the microstructure of the rubber concrete on the macroscopic strength is obtained through water conservancy, The performance prediction and improvement in the aspects of civil engineering, traffic and the like provide great help, the analysis method is scientific and rigorous, the method is in accordance with the reality, and the conclusion obtained by analysis is representative.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (6)

1. A quantitative analysis method for a microstructure of rubber concrete is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: preparation of rubber concrete samples
Cleaning a stirrer and coating slurry on the inner wall of the stirrer, sequentially adding weighed coarse aggregate, fine aggregate, rubber particles, cement and sand into the stirrer and stirring for 2 minutes, adding weighed water into the stirrer and continuously stirring for 2 minutes, unloading concrete onto a steel plate after uniform stirring and immediately carving the concrete into a test mold, then placing the test mold on a vibration table and vibrating for 1 minute, plastering the upper surface of the concrete after the concrete is formed, covering the test mold with wet cloth and standing the test mold indoors for 24 hours, and finally demolding the rubber concrete and placing the rubber concrete into a standard curing room for curing to obtain a rubber concrete sample;
step two: rubber concrete sample treatment
According to the first step, a rubber concrete sample is maintained in a standard curing room to different specified ages, after the maintenance time reaches the standard, a cutting machine is used for cutting the sample into sample blocks with the length and width of 10 x 10mm for scanning by an electron microscope and sample slices with the length and width of 100 x 15mm for analyzing a hole structure, then the sample blocks are placed in a drying oven for heating and drying treatment, the heating temperature is set to be 50 ℃, after drying, gold spraying is carried out on the observation surface of the sample blocks, then the observation surface of the sample slices is blackened, after blacking, the sample slices are placed in the drying oven for drying, after drying, a layer of white barium sulfate powder is scattered on the blackened observation surface, and the white barium sulfate powder is moved and pressed to fill the holes in the observation surface of the whole sample slices;
step three: observing the microstructure morphology of the sample cut
According to the second step, firstly, opening a scanning electron microscope system and operating control software to enable the vacuum degree of the sample chamber to return to the atmosphere, then loading the prepared sample blocks into the sample chamber and evacuating the sample chamber, then setting the parameter values of voltage, current and definition, observing the appearance of hydration products on the observation surface of the sample blocks through adjusting the multiplying power and a teaching aid, then marking the length, width and position information of microcracks on the observation surface of the sample blocks, and storing and exporting marked pictures;
step four: measurement sample section pore structure
According to the second step, measuring the geometric parameters of the pores in the observation surface of the rubber concrete sample slice by adopting a straight line wire method, firstly setting a region with the surface middle position of the observation surface of the sample slice being 50 multiplied by 50mm as an observation region, then dividing the observation region into 63 subregions with the same size and sequentially collecting the images of each subregion, wherein the number of the subregions with the same size is changed along with the area change of the total observation region, then determining a threshold value and converting the collected images into binary images so as to improve the identification effect of the pores, then measuring the number and the chord length of the pores of each subregion by adopting the straight line wire method, calculating the total number and the chord length of the pores of the whole observation region, and finally calculating the statistical value of the geometric parameters of the pores of the whole;
step five: analyzing the relationship between microstructure and macroscopic strength
According to the fourth step, firstly, a hydraulic servo universal testing machine is adopted to carry out a compressive strength test on the rubber concrete, the compressive strengths of the rubber concrete at different curing ages are compared, and then the relation between the microstructure and the macroscopic strength of the rubber concrete is obtained through analysis according to the microstructure observation result of the rubber concrete sample block and the measurement result of the rubber concrete sample block pore mechanism and by combining the compressive strength comparison results of the rubber concrete at different curing ages.
2. The quantitative analysis method for the microstructure of rubber concrete according to claim 1, wherein: in the first step, the ratio of water to cement to sand to fine aggregate to coarse aggregate to rubber particles is 2:4:5:3:8:1, the uniformly stirred concrete is cleaned by wiping the test mold before being added into the test mold, a layer of release agent is uniformly coated on the concrete, and the test mold is vibrated under pressure when vibrated on a vibration table so as to prevent the rubber particles from floating upwards.
3. The quantitative analysis method for the microstructure of rubber concrete according to claim 1, wherein: and in the second step, before the sample slice is blackened and dried, an automatic polishing machine is adopted to polish the observation surface of the sample slice, a coarse-to-fine abrasive is used for polishing in the polishing process, after polishing is finished, the residue on the surface of the sample slice is washed away by flowing clear water, and then the sample slice is put into an ultrasonic cleaning instrument for cleaning.
4. The quantitative analysis method for the microstructure of rubber concrete according to claim 1, wherein: and in the second step, spraying gold on the observation surface of the sample slice by a gold spraying instrument, keeping the current at 8mA during spraying gold, setting the gold spraying time to be 3 minutes, and repeatedly blacking the observation surface of the sample slice horizontally and vertically in sequence by a black water-based pen.
5. The quantitative analysis method for the microstructure of rubber concrete according to claim 1, wherein: in the fourth step, 63 sub-regions with the same size are composed of 7 sub-regions in the horizontal direction and 9 sub-regions in the vertical direction.
6. The quantitative analysis method for the microstructure of rubber concrete according to claim 1, wherein: in the fourth step, the calculation formula is
Figure FDA0002575295780000031
Figure FDA0002575295780000032
Figure FDA0002575295780000033
Figure FDA0002575295780000034
Wherein A is porosity, ∑ l is the sum of chord lengths of bubbles cut by the whole wire, T is the total length of the wire,
Figure FDA0002575295780000041
is the average chord length of the bubbles, n is the total number of the bubbles cut by the whole wire, r is the average radius of the bubbles,
Figure FDA0002575295780000042
is the bubble spacing coefficient, p is the slurry content in the concrete, n1The number of air bubbles cut per 10mm wire on average.
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