CN111610213B - Quantitative analysis method for microstructure of rubber concrete - Google Patents
Quantitative analysis method for microstructure of rubber concrete Download PDFInfo
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- 238000004445 quantitative analysis Methods 0.000 title claims abstract description 18
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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, processing the rubber concrete sample, observing the microstructure morphology of the cut sample, measuring the pore structure of the cut sample, and analyzing the relationship between the microstructure and the macroscopic strength; according to the invention, microstructure observation is performed on a sample block by a scanning electron microscope system, then the pore structure on a sample slice is measured by a linear wire method, and then a compressive strength test is performed on rubber concrete by a hydraulic servo universal tester, so that the influence of the microstructure of the rubber concrete on the macroscopic strength of the rubber concrete is obtained by the microstructure test and the macroscopic mechanical property test analysis, and further, great help is provided for the performance prediction and improvement of the rubber concrete in the aspects of water conservancy, civil engineering, traffic and the like.
Description
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 concrete formed by mixing, forming and curing the rubber emulsion, the auxiliary additive and the cement together when preparing cement mortar or concrete, has excellent impact resistance and wear resistance, can better solve the recycling problem of waste rubber products, has better performance in the aspects of impact resistance, crack resistance, seepage resistance, freezing resistance, shock resistance and the like compared with common concrete, can effectively reduce the use of natural aggregate and the accumulation of waste rubber products, has better application prospect in hydraulic engineering, but the strength of the rubber concrete is continuously reduced along with the increase of the rubber doping amount, and limits the engineering application of the rubber concrete to a certain extent;
in order to promote popularization and application of the rubber concrete in practical engineering such as water conservancy, civil engineering, traffic and the like, the structural strength and fracture performance of the rubber concrete are required to be analyzed to reveal a mechanism for reducing the strength of the rubber concrete and prolong the service life of a concrete structure, but the analysis of the mechanism of the strength of the rubber concrete is less at present, and the analysis result is not representative, and because the macroscopic expression of the material performance is often indistinguishable from the microstructure of the rubber concrete, the invention provides a quantitative analysis method for the microstructure of the rubber concrete to solve the problems in the prior art.
Disclosure of Invention
Aiming at the problems, the invention aims to provide a quantitative analysis method for the microstructure of the 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, micropores and the like in the rubber concrete in different ages, and analyzes the influence of the microstructure of the rubber concrete part on the macroscopic strength through a comparison 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:
step one: preparation of rubber concrete sample
Firstly cleaning a stirrer and pasting the inner wall of the stirrer, then sequentially adding weighed coarse aggregate, fine aggregate, rubber particles, cement and sand into the stirrer and stirring for 2 minutes, then adding weighed water into the stirrer and stirring for 2 minutes, unloading concrete onto a steel plate after stirring uniformly and immediately loading the steel plate into a test mould, then placing the test mould onto a vibrating table and vibrating for 1 minute, plastering the upper surface of the concrete after the concrete is formed, covering the test mould with wet cloth and standing for 24 hours indoors, and finally demoulding 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, curing a rubber concrete sample in a standard curing room to different regulated ages, cutting the sample into a sample block with the length and width of 10 multiplied by 10mm and a sample slice with the length and width of 100 multiplied by 15mm for electron microscope scanning by a cutting machine after the curing time reaches the standard, putting the sample block into a baking oven for heating and drying, setting the heating temperature to be 50 ℃, firstly spraying metal on the observation surface of the sample block after the drying is finished, then blackening the observation surface of the sample block, putting the sample block into the baking oven for drying after the blackening, scattering a layer of white barium sulfate powder on the blackened observation surface after the drying is finished, and moving and pressing to fill pores on the observation surface of the whole sample block;
step three: observing the microstructure morphology of the cut sample
According to the second step, firstly, a scanning electron microscope system is opened, the vacuum degree of a sample chamber is restored to the atmosphere by operating control software, then, the prepared sample is diced into the sample chamber, the sample chamber is evacuated, then, parameter values of voltage, current and definition are set, the shape of hydration products of a sample dicing observation surface is observed through adjusting magnification and a teaching aid, and then, the length, width and position information of microcracks on the sample dicing observation surface are marked, and the marked pictures are stored and exported;
step four: pore structure of measurement sample slice
According to the second step, a linear wire method is adopted to measure geometrical parameters of pores in a rubber concrete sample slice observation surface, firstly, an area with the size of 50 multiplied by 50mm in the middle of the surface of the sample slice observation surface is set as an observation area, then the observation area is divided into 63 subregions with the same size, images of each subregion are sequentially collected, wherein the number of subregions with the same size changes along with the area change of the total observation area, then a threshold value is determined, the collected images are converted into binary images, so that the recognition effect of the pores is improved, then the number and the chord length of pores in each subregion are measured by the linear wire method, the total number and the chord length of the pores in the whole observation area are calculated, and finally, the geometrical parameter statistical value of the pores in the whole observation area is calculated according to a formula;
step five: analysis of microstructure versus macroscopic Strength
According to the fourth step, a hydraulic servo universal tester is adopted to conduct compressive strength test on the rubber concrete, compressive strengths of the rubber concrete in different curing ages are compared, and then the relationship between the microstructure and the macroscopic strength of the rubber concrete is analyzed and obtained according to microstructure observation results of the rubber concrete sample cutting and the measurement results of the pore mechanism of the rubber concrete sample cutting and combining the compressive strength comparison results of the rubber concrete in different curing ages.
The further improvement is that: in the first step, the proportion among water, cement, sand, fine aggregate, coarse aggregate and rubber particles is 2:4:5:3:8:1, the test mould is wiped clean and uniformly coated with a layer of release agent before the uniformly stirred concrete is added into the test mould, and the test mould adopts pressurizing vibration when vibrating on a vibrating table so as to prevent the rubber particles from floating upwards.
The further improvement is that: in the second step, an automatic grinding and polishing machine is adopted to polish the observation surface of the sample slice before the sample slice is blackened and dried, a coarse-to-fine grinding material is used for polishing in the polishing process, and after polishing, flowing clean water is used for flushing off residues on the surface of the sample slice, and then the sample slice is put into an ultrasonic cleaner for cleaning.
The further improvement is that: in the second step, the observation surface of the sample block is subjected to metal spraying through a metal spraying instrument, the current is kept at 8mA during metal spraying, the metal spraying time is set to be 3 minutes, and the observation surface of the sample block is sequentially subjected to horizontal and vertical repeated blackening through a black water-based pen.
The further improvement is that: in the fourth step, 63 subregions with the same size consist of 7 subregions in the horizontal direction and 9 subregions in the vertical direction.
The further improvement is that: in the fourth step, the calculation formula is as follows
Wherein A is the porosity, sigma l is the sum of the chord lengths of the bubbles cut by the whole wire, T is the total length of the wire,
the average chord length of the bubbles is n is the total number of the bubbles cut by the whole wire, r is the average radius of the bubbles, and +>
Is the space coefficient of bubbles, p is the slurry content in the concrete, n 1 The number of bubbles cut per 10mm wire was averaged.
The beneficial effects of the invention are as follows: according to the invention, a representative rubber concrete test sample is prepared through reasonable raw material proportion, then the sample is cut, dried and subjected to metal spraying treatment according to the observation test requirement of a scanning electron microscope to obtain a sample cut block for scanning of the electron microscope, then the sample is cut, dried, blackened and subjected to barium sulfate powder scattering treatment according to the analysis test requirement of a pore structure to obtain a sample slice for pore structure analysis, then the microstructure of the sample cut block is observed through a scanning electron microscope system, the pore structure on the sample slice is measured through a linear wire method, and then the compressive strength of the rubber concrete is tested through a hydraulic servo universal tester, so that the influence of the microstructure of the rubber concrete on the macroscopic strength of the rubber concrete is obtained through the microstructure test and the macroscopic mechanical property test analysis, and the great help is provided for the performance prediction and improvement of the rubber concrete in the aspects of water conservancy, civil engineering, traffic and the like.
Drawings
FIG. 1 is a flow chart of the steps of the present invention;
FIG. 2 is a flow chart of the preparation of a rubber concrete sample according to the present invention.
Detailed Description
The present invention will be further described in detail with reference to the following examples, which are only for the purpose of illustrating the invention and are not to be construed as limiting the scope of the invention.
According to fig. 1 and 2, the embodiment provides a quantitative analysis method for a microstructure of rubber concrete, which comprises the following steps:
step one: preparation of rubber concrete sample
Wiping a test mould, uniformly coating a layer of release agent, cleaning a stirrer, coating slurry on the inner wall of the stirrer, 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 to the cement to the sand to the fine aggregate to the coarse aggregate to the rubber particles is 2:4:5:3:8:1, unloading concrete onto a steel plate after uniform stirring, immediately loading 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, demoulding the rubber concrete, and curing in a standard curing chamber to obtain a rubber concrete sample;
step two: rubber concrete sample treatment
According to the first step, curing a rubber concrete sample in a standard curing room to different specified ages, cutting the sample into a sample cut block with the length, width and height of 10 multiplied by 10mm and a sample slice with the length, width and height of 100 multiplied by 15mm for electron microscope scanning by a cutting machine after the curing time reaches the standard, putting the sample cut block into a baking oven for heating and drying treatment, setting the heating temperature to 50 ℃, spraying metal on the observation surface of the sample cut block by a metal spraying instrument after drying, keeping the current at 8mA during metal spraying time for 3 minutes, polishing the observation surface of the sample slice by an automatic polishing machine, polishing by using abrasive materials from thick to thin, flushing surface residues by flowing clear water after polishing, cleaning by an ultrasonic cleaning instrument, sequentially and repeatedly blackening the observation surface of the sample slice by a black water pen, and then scattering a layer of white barium sulfate powder on the black observation surface and moving and pressing to fill pores on the observation surface of the whole sample slice;
step three: observing the microstructure morphology of the cut sample
According to the second step, firstly, a scanning electron microscope system is opened, the vacuum degree of a sample chamber is restored to the atmosphere by operating control software, the prepared sample is diced and loaded into the sample chamber, the sample chamber is evacuated, then, parameter values of voltage, current and definition are set, the shape of hydration products of a sample dicing observation surface is observed through adjusting magnification and a teaching aid, and then, the length, width and position information of microcracks on the sample dicing observation surface are marked, and the marked pictures are stored and exported;
step four: pore structure of measurement sample slice
According to the second step, the geometrical parameters of pores in the observation surface of the rubber concrete sample slice are measured by adopting a linear wire method, firstly, an area with the size of 50 multiplied by 50mm at the middle position of the surface of the observation surface of the sample slice is set as an observation area, the observation area is divided into 63 subregions with the same size, and 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 subregions with the same size changes along with the change of the area of the total observation area, then, a threshold value is determined, the collected images are converted into binary images, so that the recognition effect of the pores is improved, then, the pore number and the chord length of each subregion are measured by adopting the linear wire method, the total pore number and the chord length of the whole observation area are calculated, and finally, the geometrical parameter statistical value of the pores of the whole observation area is calculated according to the formula, and the formula is
Wherein A is the porosity, sigma l is the sum of the chord lengths of the bubbles cut by the whole wire, T is the total length of the wire,
the average chord length of the bubbles is n is the total number of the bubbles cut by the whole wire, r is the average radius of the bubbles, and +>
Is the space coefficient of bubbles, p is the slurry content in the concrete, n 1 The number of bubbles cut per 10mm wire is averaged;
step five: analysis of microstructure versus macroscopic Strength
According to the fourth step, a hydraulic servo universal tester is adopted to conduct compressive strength test on the rubber concrete, compressive strengths of the rubber concrete in different curing ages are compared, and then the relationship between the microstructure and the macroscopic strength of the rubber concrete is analyzed and obtained according to microstructure observation results of the rubber concrete sample cutting and the measurement results of the pore mechanism of the rubber concrete sample cutting and combining the compressive strength comparison results of the rubber concrete in different curing ages.
According to the quantitative analysis method for the microstructure of the rubber concrete, a representative rubber concrete test sample is prepared through reasonable raw material proportion, then the sample is cut, dried and subjected to metal spraying according to the observation test requirement of a scanning electron microscope, so that a sample cut block for scanning of the electron microscope is obtained, then the sample is cut, dried, blackened and subjected to barium sulfate powder scattering according to the analysis test requirement of a pore structure, so that a sample slice for analyzing the pore structure is obtained, the microstructure of the sample cut block is observed through a scanning electron microscope system, the pore structure on the sample slice is measured through a linear wire method, and then the compressive strength of the rubber concrete is tested through a hydraulic servo universal tester, so that the influence of the microstructure of the rubber concrete on the macroscopic strength of the rubber concrete is obtained through the microstructure test and the macroscopic mechanical property test analysis, and the performance prediction and improvement of the rubber concrete in the aspects of water conservancy, civil engineering, traffic and the like are greatly facilitated.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (5)
1. A quantitative analysis method for a microstructure of rubber concrete is characterized by comprising the following steps: the method comprises the following steps:
step one: preparation of rubber concrete sample
Firstly cleaning a stirrer and pasting the inner wall of the stirrer, then sequentially adding weighed coarse aggregate, fine aggregate, rubber particles, cement and sand into the stirrer and stirring for 2 minutes, then adding weighed water into the stirrer and stirring for 2 minutes, unloading concrete onto a steel plate after stirring uniformly and immediately loading the steel plate into a test mould, then placing the test mould onto a vibrating table and vibrating for 1 minute, plastering the upper surface of the concrete after the concrete is formed, covering the test mould with wet cloth and standing for 24 hours indoors, and finally demoulding 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, curing a rubber concrete sample in a standard curing room to different regulated ages, cutting the sample into a sample block with the length and width of 10 multiplied by 10mm and a sample slice with the length and width of 100 multiplied by 15mm for electron microscope scanning by a cutting machine after the curing time reaches the standard, putting the sample block into a baking oven for heating and drying, setting the heating temperature to be 50 ℃, firstly spraying metal on the observation surface of the sample block after the drying is finished, then blackening the observation surface of the sample block, putting the sample block into the baking oven for drying after the blackening, scattering a layer of white barium sulfate powder on the blackened observation surface after the drying is finished, and moving and pressing to fill pores on the observation surface of the whole sample block;
step three: observing the microstructure morphology of the cut sample
According to the second step, firstly, a scanning electron microscope system is opened, control software is operated to restore the vacuum degree of a sample chamber to the atmosphere, then, the prepared sample is diced into the sample chamber, the sample chamber is evacuated, then, parameter values of voltage, current and definition are set, the shape of hydration products of a sample dicing observation surface is observed through adjusting magnification and a teaching aid, and then, the length, width and position information of microcracks on the sample dicing observation surface are marked, and the marked pictures are stored and exported;
step four: pore structure of measurement sample slice
According to the second step, a linear wire method is adopted to measure geometrical parameters of pores in a rubber concrete sample slice observation surface, firstly, an area with the size of 50 multiplied by 50mm in the middle of the surface of the sample slice observation surface is set as an observation area, then the observation area is divided into 63 subregions with the same size, images of each subregion are sequentially collected, wherein the number of subregions with the same size changes along with the area change of the total observation area, then a threshold value is determined, the collected images are converted into binary images, so that the pore identification effect is improved, then the number and the chord length of pores in each subregion are measured by the linear wire method, the total number and the chord length of pores in the whole observation area are calculated, and finally, the geometrical parameter statistical value of the pores in the whole observation area is calculated according to a formula;
in the fourth step, 63 subregions with the same size consist of 7 subregions in the horizontal direction and 9 subregions in the vertical direction;
step five: analysis of microstructure versus macroscopic Strength
According to the fourth step, a hydraulic servo universal tester is adopted to conduct compressive strength test on the rubber concrete, compressive strengths of the rubber concrete in different curing ages are compared, and then the relationship between the microstructure and the macroscopic strength of the rubber concrete is analyzed according to microstructure observation results of the rubber concrete sample cutting and pore structure measurement results of the rubber concrete sample cutting and by combining the compressive strength comparison results of the rubber concrete in different curing ages.
2. The quantitative analysis method for the microstructure of the rubber concrete according to claim 1, wherein the quantitative analysis method comprises the following steps of: in the first step, the proportion among water, cement, sand, fine aggregate, coarse aggregate and rubber particles is 2:4:5:3:8:1, the test mould is wiped clean and uniformly coated with a layer of release agent before the uniformly stirred concrete is added into the test mould, and the test mould adopts pressurizing vibration when vibrating on a vibrating table so as to prevent the rubber particles from floating upwards.
3. The quantitative analysis method for the microstructure of the rubber concrete according to claim 1, wherein the quantitative analysis method comprises the following steps of: in the second step, an automatic grinding and polishing machine is adopted to polish the observation surface of the sample slice before the sample slice is blackened and dried, a coarse-to-fine grinding material is used for polishing in the polishing process, and after polishing, flowing clean water is used for flushing off residues on the surface of the sample slice, and then the sample slice is put into an ultrasonic cleaner for cleaning.
4. The quantitative analysis method for the microstructure of the rubber concrete according to claim 1, wherein the quantitative analysis method comprises the following steps of: in the second step, the observation surface of the sample block is subjected to metal spraying through a metal spraying instrument, the current is kept at 8mA during metal spraying, the metal spraying time is set to be 3 minutes, and the observation surface of the sample block is sequentially subjected to horizontal and vertical repeated blackening through a black water-based pen.
5. The quantitative analysis method for the microstructure of the rubber concrete according to claim 1, wherein the quantitative analysis method comprises the following steps of: in the fourth step, the calculation formula is as follows
Wherein A is porosity and Σl is fullThe sum of the chord lengths of the bubbles cut by the lead, T is the total length of the lead,
the average chord length of the bubbles is n is the total number of the bubbles cut by the whole wire, r is the average radius of the bubbles, and +.>
Is the space coefficient of bubbles, p is the slurry content in the concrete, n 1 The number of bubbles cut per 10mm wire was averaged. />
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