CN117007395A - Preparation method of microscopic analysis sample of ultra-high-performance concrete - Google Patents

Preparation method of microscopic analysis sample of ultra-high-performance concrete Download PDF

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Publication number
CN117007395A
CN117007395A CN202310943079.0A CN202310943079A CN117007395A CN 117007395 A CN117007395 A CN 117007395A CN 202310943079 A CN202310943079 A CN 202310943079A CN 117007395 A CN117007395 A CN 117007395A
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tested
sample
polishing
ultra
performance concrete
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李叶青
饶梅
万大伟
石春芝
余松柏
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Huaxin Cement Co Ltd
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Huaxin Cement Co Ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/30—Staining; Impregnating ; Fixation; Dehydration; Multistep processes for preparing samples of tissue, cell or nucleic acid material and the like for analysis
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/32—Polishing; Etching
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34—Purifying; Cleaning
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/36—Embedding or analogous mounting of samples
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • G01N2001/2873—Cutting or cleaving
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/36—Embedding or analogous mounting of samples
    • G01N2001/364—Embedding or analogous mounting of samples using resins, epoxy
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/91—Use of waste materials as fillers for mortars or concrete

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
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  • Engineering & Computer Science (AREA)
  • Biomedical Technology (AREA)
  • Molecular Biology (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The invention discloses a preparation method of a microscopic analysis sample of ultra-high-performance concrete. The method comprises the following steps: cutting, hydration termination, rough grinding, fine grinding, polishing, cleaning and drying the ultra-high performance concrete to prepare an ultra-high performance concrete microscopic analysis sample, and vacuum sealing; wherein: soaking with alcohol after hydration, coarse grinding with 1000 mesh sand paper, fine grinding with 2000 mesh sand paper, 3000 mesh sand paper and 5000 mesh sand paper successively, and polishing with silk polishing cloth. The ultra-high concrete microscopic analysis sample obtained by the preparation method has the advantages of flat and smooth surface, complete structure, excellent quality, long-time storage of the sample, scientific flow, simple process and wide application prospect.

Description

Preparation method of microscopic analysis sample of ultra-high-performance concrete
Technical Field
The invention belongs to the field of building material test analysis, and particularly relates to a preparation method of an ultra-high performance concrete microscopic analysis sample.
Background
The ultra-high performance concrete is used as an innovative cement-based engineering material, has ultra-high compressive strength and excellent durability, and has extremely high advantages and wide application prospects in the fields of high-rise buildings, building decorations, bridge structures, explosion-proof engineering, repair reinforcement and the like. But the performance of ultra-high performance concrete is further optimized by adopting the traditional method, and the bottleneck period is already entered. With the vigorous development of a material microstructure test method, people pay more attention to the microstructure and micromechanics of ultra-high-performance concrete, microstructure detection comprises scanning electron microscope SEM and electron probe EPMA, and the optimization of the service performance of the material is guided by deep knowledge of the internal structural characteristics of the material, so that the method has important significance for expanding wider application of the material.
Microscopic testing of ultra-high performance concrete includes: scanning electron microscopy scanning electron images SEM, back scattering images BSE, electron probes EPMA, microhardness, nanoindentation, etc. These microscopic test analyses require the preparation of interfaces with smooth surfaces and high flatness. The ultra-high performance concrete contains gel, clinker, aggregate and other admixtures, the hardness of each phase is obviously different, and in general, the hardness is ordered from large to small: aggregate > clinker ≡ admixture > gel, and the aggregate which is adopted by the ultra-high performance concrete with different strength grades is: carborundum, quartz sand, river sand and machine-made sand, wherein the hardness of the aggregate is ranked from large to small: emery > quartz sand > river sand > machine-made sand. In order to prepare a smooth interface of ultra-high performance concrete in the process of preparing a microscopic analysis sample, the softer phase C-S-H gel is easy to be subjected to overpolish, so that the problem of obvious unevenness of an aggregate-gel interface or a fiber-gel surface is caused, and the subsequent microscopic structure and microscopic mechanical property test are influenced.
Disclosure of Invention
The invention aims to provide a preparation method of an ultra-high performance concrete microscopic analysis sample, wherein the obtained ultra-high performance concrete microscopic analysis sample has the advantages of flat and smooth surface, complete structure, excellent quality, long-time storage of the sample, scientific flow, simple process and wide application prospect.
In order to solve the technical problems, the invention adopts the following technical scheme:
the preparation and preservation method of the microscopic analysis sample of the ultra-high performance concrete comprises the following steps:
1) Cutting: cutting the ultra-high performance concrete test block to be tested into blocks by using a precise diamond cutting machine, exposing a fresh surface to be tested, and obtaining a block to be tested;
2) Terminating hydration: soaking the block to be tested obtained in the step 1) in alcohol, taking out, soaking in fresh alcohol, repeating for 4-5 times, and vacuum drying;
3) Rough polishing: coarsely polishing the surface to be tested of the sample for 20-60 s until the surface to be tested is smooth at the speed of 100-150 r/min by using 1000-mesh SiC sand paper; coarsely polishing the surface to be measured at a speed of 100-150 r/min until the surface to be measured is parallel to the upper and lower surfaces as much as possible;
4) And (3) fine grinding: finely grinding the block to be tested after the rough grinding in the step 3), wherein SiC sand paper with 2000 meshes, 3000 meshes and 5000 meshes is sequentially used, and the surface to be tested of the sample is respectively ground for 2-5 min at the pressure of 5-10N and the speed of 100-150 r/min;
5) Polishing: polishing the block to be tested after the fine grinding in the step 4), wherein silk polishing cloth is adopted to polish the surface to be tested of the sample for 30-90 s at a pressure of 5-10N and a speed of 50-100 r/min;
6) And (5) cleaning and drying: and 5) cleaning the polished block to be tested in the step 5) by using absolute ethyl alcohol, drying to obtain an ultra-high performance concrete microscopic analysis sample, and preserving in vacuum.
According to the above scheme, in the step 1), the aggregate in the ultra-high performance concrete raw material is one or more of machine-made sand, quartz sand, river sand and silicon carbide.
According to the scheme, in the step 1), the block to be tested is in the shape of a cube, a cylinder or other irregular blocks, wherein the thickness of the sample to be tested is 1-20 mm, and the maximum length, width or diameter is less than or equal to 45mm.
According to the above scheme, in the step 2), the alcohol is absolute ethanol or isopropanol.
According to the scheme, in the step 2), the soaking time of the block to be tested in alcohol is 3-5 h; the vacuum drying conditions are as follows: vacuum degree of vacuum drying is less than or equal to 133Pa, and drying time is 20-30 min.
According to the scheme, in the step 3), absolute ethyl alcohol is used as a lubricant; preferably, the lubricant addition rate is 2 to 10mL/min.
According to the scheme, in the step 3), the side of the surface to be detected is roughly polished for 2-4 min.
According to the scheme, in the step 4), an automatic polishing machine is adopted for fine polishing.
According to the scheme, in the step 4), absolute ethyl alcohol is used as a lubricant; preferably, the lubricant addition rate is 2 to 10mL/min.
According to the scheme, in the step 5), an automatic polishing machine is adopted for polishing.
According to the scheme, in the step 5), absolute ethyl alcohol is used as a lubricant; preferably, the lubricant addition rate is 2 to 10mL/min.
According to the scheme, in the step 5), polishing solution with the particle size of 0.05-0.5 microns is sprayed on the polishing cloth; preferably, the polishing liquid is an alumina or diamond polishing liquid.
According to the above scheme, in the step 6), the block to be tested is placed in absolute ethyl alcohol with the face facing upwards, the block to be tested is placed in an ultrasonic cleaner, the block to be tested is cleaned for 3-8 min by ultrasonic, the sample to be tested is taken out, and the sample is dried by inert air flow, so that the ultra-high performance concrete microscopic analysis sample is obtained.
According to the above scheme, in the step 6), vacuum preservation is as follows: wrapping the block to be tested with dust-free paper, filling into a clean vacuum packaging bag, and then placing into a vacuum packaging machine for vacuum packaging and preservation.
According to the scheme, when the age of the ultra-high performance concrete to be tested is less than or equal to 12 hours, the method further comprises the steps of dipping and embedding, and specifically comprises the following steps: placing the block to be tested after hydration termination in the step 2) into a silica gel mold, enabling the surface to be tested of the sample to be in contact with the bottom surface of the silica gel test mold, pouring the liquid curing agent into the silica gel test mold until the top of the sample is submerged, and standing the silica gel test mold until the curing agent is completely cured; wherein the liquid curing agent is epoxy resin or acrylic, the standing time is 3-8 h, and the acrylic is 20-30 min;
preferably, the silica gel mold is in a cube or cylinder shape, the thickness of the mold is 20-40 mm, and the maximum length, width or diameter is less than or equal to 50mm.
In order to obtain an ultra-high performance concrete interface with smooth surface and high flatness, the invention adopts the following process:
firstly, cutting ultra-high performance concrete by adopting a precise diamond cutting machine, wherein the cutting surface is smooth and flat, and the damage layer is far smaller than that of a common concrete cutting machine; then, rough grinding is carried out by using 1000-mesh SiC sand paper, the mesh is small and fine, and secondary damage is avoided when the surface damage left on the surface to be measured by the precise diamond cutting machine is ground; then sequentially carrying out fine grinding by using small pressures of 2000-mesh, 3000-mesh and 5000-mesh SiC sand paper, further flattening the interface and simultaneously providing powerful guarantee for subsequent rapid polishing and achieving good polishing effect. Finally, quick polishing is carried out under small pressure by adopting silk polishing cloth, so that the surface to be tested is guaranteed to be polished to a mirror surface, and the phenomenon of over-polishing caused by long polishing time of soft phase C-S-H gel is prevented; meanwhile, the silk polishing cloth is also the key for ensuring plane polishing, and compared with other polishing cloths (velvet, nylon, imported velvet and the like), the silk polishing cloth has no velvet and has polishing of materials with different hardness phases.
The beneficial effects of the invention are as follows:
1. the invention provides a preparation method of a microscopic analysis sample of ultra-high performance concrete, which adopts a precise diamond cutting machine for cutting, and has small damage layer; the microstructure of the sample at a specific age can be reserved by matching with alcohol soaking to terminate hydration; and then, by cooperating with 1000-mesh rapid rough grinding, 2000-mesh, 3000-mesh and 5000-mesh long-time low-pressure fine grinding and rapid silk polishing processes, the phenomenon of over-polishing of softer phase C-S-H gel is greatly reduced, the surface roughness of an aggregate-gel interface is obviously improved, the surface roughness Sa is less than 800nm, the microstructure and micromechanics test analysis are completely satisfied, the process is scientific, the process is simple and convenient, and the method has wide application prospect.
2. Further, because the strength of the ultra-high performance concrete with the age less than or equal to 12 hours is extremely low, the test block is not formed and fragile, the test block is impregnated and embedded after hydration is stopped, and then precise diamond cutting, grinding and polishing are carried out, so that the complete structure of the test block can be ensured, and the guarantee is provided for the follow-up accurate microstructure and micromechanics test analysis.
3. According to the invention, the sample is stored by vacuum encapsulation, so that hydration and carbonization of the surface to be tested and air are effectively prevented, and the sample is convenient for long-term storage.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a photograph of a quartz sand aggregate ultra-high performance concrete microscopic analysis sample prepared in example 1 of the present invention on a scale of 50 μm under reflected light.
Fig. 2 is a 3D profile photograph of the surface of a microscopic analysis sample of the ultra-high performance concrete of the quartz sand aggregate prepared in example 1 of the present invention.
FIG. 3 is a line profile photograph of a microscopic analysis sample of the ultra-high performance concrete of quartz sand aggregate prepared in example 1 of the present invention.
FIG. 4 is a photograph of a quartz sand aggregate ultra-high performance concrete microscopic analysis specimen of comparative example 1 on a scale of 50 μm under reflected light.
Fig. 5 is a photograph of a 3D profile of the surface of a sample of the ultra-high performance concrete microscopic analysis of the quartz sand aggregate of comparative example 1.
FIG. 6 is a photograph of the surface line profile of a sample of the ultra-high performance concrete microscopic analysis of the quartz sand aggregate of comparative example 1.
FIG. 7 is a photograph of a quartz sand aggregate ultra-high performance concrete microscopic analysis specimen of comparative example 2 on a scale of 50 μm under reflected light.
FIG. 8 is a photograph of a 20 μm ruler under SEM secondary electrons after 1 month of preservation of a quartz sand aggregate ultra-high performance concrete microscopic analysis sample preparation according to example 1 of the present invention.
FIG. 9 is a photograph of a scale of 50 μm under SEM secondary electrons after 1 month of storage of comparative example 2 quartz sand aggregate ultra-high performance concrete microscopic analysis sample preparation.
Fig. 10 is a photograph of a sample of ultra-high performance concrete (age 6 hours) of the corundum aggregate of example 5 of the present invention (a) after termination of hydration (b) after immersion inlay polishing.
Detailed Description
The following examples further illustrate the present invention, but are not limited thereto.
The raw materials used in the examples and comparative examples of the present invention are all conventional raw materials and commercially available.
Example 1
The preparation method of the quartz sand aggregate ultra-high performance concrete analysis sample comprises the following steps:
(1) Cutting: cutting the quartz sand aggregate ultra-high performance concrete test block into blocks by using a precise diamond cutting machine to expose a fresh surface to be tested, wherein the length and width of the block to be tested are 10mm multiplied by 10mm, and the thickness of the block to be tested is 10mm;
(2) Terminating hydration: soaking the sample cut in the step (1) with absolute ethyl alcohol for 3 hours, taking out the sample, soaking the sample in fresh absolute ethyl alcohol for 3 hours, repeating the step for 4 times, taking out the sample, and placing the sample in a vacuum drying oven for drying, wherein the vacuum degree is less than or equal to 133Pa, and the drying time is 20 minutes;
(3) Rough polishing: taking out the sample immersed and embedded and solidified in the step (2), and using 1000-mesh SiC sand paper to coarsely polish the surface to be tested of the sample at the speed of 100r/min for 30s until the surface is smooth; coarsely polishing the opposite side 4 mm of the surface to be detected at the speed of 150r/min, wherein the upper surface and the lower surface are as parallel as possible; absolute ethyl alcohol is used as a lubricant, and the dropping speed of the lubricant is 10ml/min;
(4) And (3) fine grinding: adopting an automatic polishing machine to polish the surface to be tested of the sample in the step (3) by fixing the surface to be tested on a polishing clamp with the downward facing direction, and polishing the surface to be tested of the sample for 2min by using 2000-mesh SiC sand paper, 10N pressure of a pressing head, 60r/min rotating speed of the clamp and 150r/min rotating speed of a rotating disc (the rotating disc of the clamp rotates in the same direction); polishing a surface to be detected of a sample for 2min by using 3000-mesh SiC sand paper, 5N pressure of a pressure head, 60r/min rotating speed of a clamp and 100r/min rotating speed of a turntable (the clamp turntable rotates in the same direction); polishing a surface to be detected of a sample for 5min by using 5000-mesh SiC sand paper, 5N pressure of a pressure head, 60r/min rotating speed of a clamp and 100r/min rotating speed of a turntable (the clamp turntable rotates in the same direction); absolute ethyl alcohol is used as a lubricant, and the dropping speed of the lubricant is 10ml/min;
(5) Polishing: adopting an automatic polishing machine to polish the surface to be tested of the sample in the step (4) by adopting an automatic polishing machine, fixing the surface to be tested on a polishing clamp, adopting silk polishing cloth, spraying alumina polishing solution with the grain diameter of 0.5 micrometer on the polishing cloth, and polishing the surface to be tested of the sample for 30s at the speed of 5N pressure, 10r/min rotating speed of the clamp and 50r/min (the clamp rotating disk rotates in the same direction), wherein absolute ethyl alcohol is used as a lubricant, and the dropping speed of the lubricant is 2ml/min; the method comprises the steps of carrying out a first treatment on the surface of the
(6) And (5) cleaning and drying: placing the polished sample to be tested in the step (5) with the surface facing upwards, placing the sample to be tested in a beaker filled with absolute ethyl alcohol, placing the beaker in an ultrasonic cleaner, ultrasonically cleaning for 3min, taking out the sample to be tested, and drying the sample by inert gas flow to obtain a quartz sand aggregate ultra-high performance concrete microscopic analysis sample;
(7) Vacuum sealing: wrapping the sample to be tested after cleaning and drying in the step (6) by dust-free paper, filling the sample into a clean vacuum packaging bag, and then placing the bag into a vacuum packaging machine for vacuum packaging and preservation.
Example 2
The preparation method of the machine-made sand aggregate ultra-high performance concrete analysis sample comprises the following steps:
(1) Cutting: cutting the machine-made sand aggregate ultra-high performance concrete test block into blocks by a precise diamond cutting machine to expose a fresh surface to be tested, wherein the length and width of the block to be tested are 20mm multiplied by 20mm, and the thickness of the block to be tested is 3mm;
(2) Terminating hydration: soaking the sample cut in the step (1) with absolute ethyl alcohol for 5 hours, taking out the sample, soaking the sample in fresh absolute ethyl alcohol for 5 hours, repeating the step for 5 times, taking out the sample, and placing the sample in a vacuum drying oven for drying, wherein the vacuum degree is less than or equal to 133Pa, and the drying time is 30 minutes;
(3) Rough polishing: taking out the sample immersed and inlaid and cured in the step (2), and using 1000-mesh SiC sand paper to coarsely polish the surface to be tested of the sample at the speed of 100r/min for 30s until the curing agent layer is removed, so that the surface is smooth; coarsely polishing the opposite side of the surface to be detected at the speed of 150r/min for 2min, wherein the upper surface and the lower surface are as parallel as possible; absolute ethyl alcohol is used as a lubricant, and the dropping speed of the lubricant is 10ml/min;
(4) And (3) fine grinding: adopting an automatic polishing machine to polish the surface to be tested of the sample in the step (3) by fixing the surface to be tested on a polishing clamp with the downward facing direction, and polishing the surface to be tested of the sample for 2min by using 2000-mesh SiC sand paper, 5N pressure of a pressing head, 60r/min rotating speed of the clamp and 150r/min rotating speed of a rotating disc (the rotating disc of the clamp rotates in the same direction); polishing a surface to be detected of a sample for 2min by using 3000-mesh SiC sand paper, 5N pressure of a pressure head, 60r/min rotating speed of a clamp and 100r/min rotating speed of a turntable (the clamp turntable rotates in the same direction); polishing a surface to be detected of a sample for 3min by using 5000-mesh SiC sand paper, 5N pressure of a pressure head, 60r/min rotating speed of a clamp and 100r/min rotating speed of a turntable (the clamp turntable rotates in the same direction); absolute ethyl alcohol is used as a lubricant, and the dropping speed of the lubricant is 10ml/min;
(5) Polishing: adopting an automatic polishing machine to polish the surface to be tested of the sample in the step (4) by adopting an automatic polishing machine, fixing the surface to be tested on a polishing clamp, adopting silk polishing cloth, spraying alumina polishing solution with the grain diameter of 0.5 micrometer on the polishing cloth, and polishing the surface to be tested of the sample for 30s at the speed of 5N pressure, 10r/min rotating speed of the clamp and 50r/min (the clamp rotating disk rotates in the same direction), wherein absolute ethyl alcohol is used as a lubricant, and the dropping speed of the lubricant is 2ml/min; the method comprises the steps of carrying out a first treatment on the surface of the
(6) And (5) cleaning and drying: placing the polished sample to be tested in the step (5) with the surface facing upwards, placing the sample to be tested in a beaker filled with absolute ethyl alcohol, placing the beaker in an ultrasonic cleaning machine, ultrasonically cleaning for 8min, taking out the sample to be tested, and drying the sample by inert gas flow to obtain a quartz sand aggregate ultra-high performance concrete microscopic analysis sample;
(7) Vacuum sealing: wrapping the sample to be tested after cleaning and drying in the step (6) by dust-free paper, filling the sample into a clean vacuum packaging bag, and then placing the bag into a vacuum packaging machine for vacuum packaging and preservation.
Example 3
The preparation method of the diamond aggregate ultra-high performance concrete analysis sample comprises the following steps:
(1) Cutting: cutting the ultra-high performance concrete test block of the diamond aggregate into blocks by a precise diamond cutting machine to expose a fresh surface to be tested, wherein the length and width of the block to be tested are 20mm multiplied by 20mm, and the thickness of the block to be tested is 5mm;
(2) Terminating hydration: soaking the sample cut in the step (1) with absolute ethyl alcohol for 5 hours, taking out the sample, soaking the sample in fresh absolute ethyl alcohol for 5 hours, repeating the step for 5 times, taking out the sample, and placing the sample in a vacuum drying oven for drying, wherein the vacuum degree is less than or equal to 133Pa, and the drying time is 30 minutes;
(3) Rough polishing: taking out the sample immersed and inlaid and cured in the step (2), and using 1000-mesh SiC sand paper to coarsely polish the surface to be tested of the sample at the speed of 150r/min for 60s until the curing agent layer is removed, so that the surface is smooth; coarsely polishing the opposite side of the surface to be detected at the speed of 150r/min for 5min, wherein the upper surface and the lower surface are as parallel as possible; absolute ethyl alcohol is used as a lubricant, and the dropping speed of the lubricant is 10ml/min;
(4) And (3) fine grinding: adopting an automatic polishing machine to polish the surface to be tested of the sample in the step (3) by fixing the surface to be tested on a polishing clamp with the surface to be tested facing downwards and using 2000-mesh SiC sand paper, 10N pressure of a pressing head, 60r/min rotating speed of the clamp and 150r/min rotating speed of a rotating disc (the rotating disc of the clamp rotates in the same direction); polishing a surface to be measured of a sample for 4min by using 3000-mesh SiC sand paper, 10N pressure of a pressure head, 60r/min rotating speed of a clamp and 100r/min rotating speed of a turntable (the clamp turntable rotates in the same direction); polishing a surface to be measured of a sample for 4min by using 5000-mesh SiC sand paper, 10N pressure of a pressure head, 60r/min rotating speed of a clamp and 100r/min rotating speed of a turntable (the clamp turntable rotates in the same direction); absolute ethyl alcohol is used as a lubricant, and the dropping speed of the lubricant is 10ml/min;
(5) Polishing: adopting an automatic polishing machine to polish the surface to be tested of the sample in the step (4) by adopting an automatic polishing machine, fixing the surface to be tested on a polishing clamp, adopting silk polishing cloth, spraying alumina polishing solution with the grain diameter of 0.5 micrometer on the polishing cloth, and polishing the surface to be tested of the sample for 30s at the speed of 5N pressure, 10r/min rotating speed of the clamp and 50r/min (the clamp rotating disk rotates in the same direction), wherein absolute ethyl alcohol is used as a lubricant, and the dropping speed of the lubricant is 2ml/min; the method comprises the steps of carrying out a first treatment on the surface of the
(6) And (5) cleaning and drying: placing the polished sample to be tested in the step (5) with the surface facing upwards, placing the sample to be tested in a beaker filled with absolute ethyl alcohol, placing the beaker in an ultrasonic cleaning machine, ultrasonically cleaning for 5min, taking out the sample to be tested, and drying the sample by inert gas flow to obtain a quartz sand aggregate ultra-high performance concrete microscopic analysis sample;
(7) Vacuum sealing: wrapping the sample to be tested after cleaning and drying in the step (6) by dust-free paper, filling the sample into a clean vacuum packaging bag, and then placing the bag into a vacuum packaging machine for vacuum packaging and preservation.
Example 4
The preparation method of the river sand aggregate ultra-high performance concrete analysis sample comprises the following steps:
(1) Cutting: cutting the river sand aggregate ultra-high performance concrete test block into blocks by a precise diamond cutting machine to expose a fresh surface to be tested, wherein the length and width of the block to be tested are 10mm multiplied by 20mm, and the thickness of the block to be tested is 15mm;
(2) Terminating hydration: soaking the sample cut in the step (1) with absolute ethyl alcohol for 5 hours, taking out the sample, soaking the sample in fresh absolute ethyl alcohol for 5 hours, repeating the step for 5 times, taking out the sample, and placing the sample in a vacuum drying oven for drying, wherein the vacuum degree is less than or equal to 133Pa, and the drying time is 30 minutes;
(3) Rough polishing: taking out the sample immersed and inlaid and cured in the step (3), and using 1000-mesh SiC sand paper to coarsely polish the surface to be tested of the sample at the speed of 120r/min for 30s until the curing agent layer is removed, so that the surface is smooth; coarsely polishing the opposite side of the surface to be detected at the speed of 120r/min for 3min, wherein the upper surface and the lower surface are as parallel as possible; absolute ethyl alcohol is used as a lubricant, and the dropping speed of the lubricant is 10ml/min;
(4) And (3) fine grinding: adopting an automatic polishing machine to polish the surface to be tested of the sample in the step (3) by fixing the surface to be tested on a polishing clamp with downward facing, and polishing the surface to be tested of the sample for 3min by using 2000-mesh SiC sand paper, 5N pressure of a pressing head, 60r/min rotating speed of the clamp and 150r/min rotating speed of a rotating disc (the rotating disc of the clamp rotates in the same direction); polishing a surface to be measured of a sample for 4min by using 3000-mesh SiC sand paper, 5N pressure of a pressure head, 60r/min rotating speed of a clamp and 100r/min rotating speed of a turntable (the clamp turntable rotates in the same direction); polishing a surface to be detected of a sample for 4min by using 5000-mesh SiC sand paper, 5N pressure of a pressure head, 60r/min rotating speed of a clamp and 100r/min rotating speed of a turntable (the clamp turntable rotates in the same direction); absolute ethyl alcohol is used as a lubricant, and the dropping speed of the lubricant is 10ml/min;
(5) Polishing: adopting an automatic polishing machine to polish the surface to be tested of the sample in the step (4) by adopting an automatic polishing machine, fixing the surface to be tested on a polishing clamp, adopting silk polishing cloth, spraying diamond polishing liquid with the grain diameter of 0.5 micrometer on the polishing cloth, and polishing the surface to be tested of the sample for 30s at the speed of 5N pressure, the rotating speed of 10r/min of the clamp and the rotating speed of 50r/min of a rotating disc (the rotating disc of the clamp rotates in the same direction), wherein absolute ethyl alcohol is used as a lubricant, and the dropping speed of the lubricant is 5ml/min; the method comprises the steps of carrying out a first treatment on the surface of the
(6) And (5) cleaning and drying: placing the polished sample to be tested in the step (5) with the surface facing upwards, placing the sample to be tested in a beaker filled with absolute ethyl alcohol, placing the beaker in an ultrasonic cleaning machine, ultrasonically cleaning for 4min, taking out the sample to be tested, and drying the sample by inert gas flow to obtain a quartz sand aggregate ultra-high performance concrete microscopic analysis sample;
(7) Vacuum sealing: wrapping the sample to be tested after cleaning and drying in the step (6) by dust-free paper, filling the sample into a clean vacuum packaging bag, and then placing the bag into a vacuum packaging machine for vacuum packaging and preservation.
The polished surfaces of the ultra-high performance concrete microscopic analysis samples of examples 1 to 4 and comparative examples 1 and 2 were subjected to structural evaluation, and test analysis according to GB/T10610-2009 rules and methods for evaluating surface structures by the product geometry technical Specification (GPS) surface Structure Profile method.
Example 5
The preparation method of the carborundum aggregate ultra-high performance concrete analysis sample with the age of 6 hours comprises the following steps:
(1) Terminating hydration: taking a carborundum aggregate ultra-high performance concrete sample with an age of 6 hours, soaking the sample in absolute ethyl alcohol for 3 hours, taking out the sample, soaking the sample in fresh absolute ethyl alcohol for 3 hours, repeating the step for 4 times, taking out the sample, and placing the sample in a vacuum drying oven for drying, wherein the vacuum degree is less than or equal to 133Pa, and the drying time is 20 minutes;
(2) Placing the sample with hydration termination in the step (1) into a silica gel mold with a clean diameter of 25mm, enabling a surface to be tested of the sample to contact with the bottom surface of the silica gel mold, pouring liquid acrylic into the silica gel mold until the top of the sample is submerged, and standing the silica gel mold for 30min until the acrylic is completely solidified;
(3) Cutting: cutting the mosaic blocks by a precise diamond cutting machine to expose a fresh surface to be measured, wherein the diameter to be measured is 25mm, and the thickness is 13mm;
(4) Rough polishing: taking out the sample in the step (3), and using 1000-mesh SiC sand paper to coarsely polish the surface to be tested of the sample at the speed of 100r/min for 30s until the surface is smooth; coarsely polishing the opposite side 2 mm of the surface to be detected at the speed of 150r/min, wherein the upper surface and the lower surface are as parallel as possible; absolute ethyl alcohol is used as a lubricant, and the dropping speed of the lubricant is 10ml/min;
(5) And (3) fine grinding: adopting an automatic polishing machine to polish the surface to be tested of the sample in the step (4) by fixing the surface to be tested on a polishing clamp with the downward facing direction, and polishing the surface to be tested of the sample for 2min by using 2000-mesh SiC sand paper, 10N pressure of a pressing head, 60r/min rotating speed of the clamp and 150r/min rotating speed of a rotating disc (the rotating disc of the clamp rotates in the same direction); polishing a surface to be detected of a sample for 2min by using 3000-mesh SiC sand paper, 5N pressure of a pressure head, 60r/min rotating speed of a clamp and 100r/min rotating speed of a turntable (the clamp turntable rotates in the same direction); polishing a surface to be detected of a sample for 5min by using 5000-mesh SiC sand paper, 5N pressure of a pressure head, 60r/min rotating speed of a clamp and 100r/min rotating speed of a turntable (the clamp turntable rotates in the same direction); absolute ethyl alcohol is used as a lubricant, and the dropping speed of the lubricant is 10ml/min;
(6) Polishing: adopting an automatic polishing machine to polish the surface to be tested of the sample in the step (5) by adopting an automatic polishing machine, fixing the surface to be tested on a polishing clamp, adopting silk polishing cloth, spraying alumina polishing solution with the grain diameter of 0.5 micrometer on the polishing cloth, and polishing the surface to be tested of the sample for 30s at the speed of 5N pressure, 10r/min rotating speed of the clamp and 50r/min (the clamp rotating disk rotates in the same direction), wherein absolute ethyl alcohol is used as a lubricant, and the dropping speed of the lubricant is 2ml/min; the method comprises the steps of carrying out a first treatment on the surface of the
(7) And (5) cleaning and drying: placing the polished sample to be tested in the step (6) with the surface facing upwards, placing the sample to be tested in a beaker filled with absolute ethyl alcohol, placing the beaker in an ultrasonic cleaner, ultrasonically cleaning for 3min, taking out the sample to be tested, and drying the sample by inert gas flow to obtain a quartz sand aggregate ultra-high performance concrete microscopic analysis sample;
(8) Vacuum sealing: and (3) wrapping the sample to be tested after cleaning and drying in the step (7) by dust-free paper, filling the sample into a clean vacuum packaging bag, and then placing the bag into a vacuum packaging machine for vacuum packaging and preservation.
Comparative example 1
Cutting the microscopic analysis sample of the quartz sand ultra-high performance concrete provided by the comparative example by adopting a precise diamond cutting machine to expose a fresh surface to be tested, wherein the length and width of the block to be tested are 10mm multiplied by 10mm, and the thickness is 10mm;
soaking in absolute ethyl alcohol to terminate hydration, and drying in a vacuum drying oven for 20min with vacuum degree of less than or equal to 133 Pa; coarsely polishing the surface to be detected of the sample for 5min at a speed of 200r/min by using 400-mesh SiC sand paper; polishing a surface to be detected of a sample for 5min by using 1000-mesh SiC sand paper, 15N pressure of a pressure head, 100r/min rotating speed of a clamp and 150r/min rotating speed of a turntable; polishing a surface to be measured of a sample for 5min by using 2000-mesh SiC sand paper, 5N pressure of a pressure head, 60r/min rotating speed of a clamp and 150r/min rotating speed of a turntable (the clamp turntable rotates in the same direction); and (3) adopting an automatic polishing machine, fixing the surface to be tested on a polishing clamp with the surface to be tested facing downwards, adopting velvet polishing cloth, spraying alumina polishing solution with the particle size of 0.5 microns on the polishing cloth, polishing the surface to be tested of the sample for 5min at the speed of 50r/min of a rotating disc (the rotating disc of the clamp rotates in the opposite direction) with the rotating speed of 100r/min of the clamp, taking absolute ethyl alcohol as a lubricant, enabling the dropping speed of the lubricant to be 2ml/min, obtaining a microscopic analysis sample, and drying and storing.
Comparative example 2
The quartz sand ultra-high performance concrete microscopic analysis sample provided by the comparative example is cut by a common cutting machine to expose a fresh surface to be tested, wherein the length and width of the block to be tested are 10mm multiplied by 10mm, and the thickness is 10mm;
soaking in absolute ethyl alcohol to terminate hydration, and drying in a vacuum drying oven for 20min with vacuum degree of less than or equal to 133 Pa; coarsely polishing the surface to be detected of the sample for 5min at a speed of 200r/min by using 400-mesh SiC sand paper; polishing a surface to be detected of a sample for 5min by using 1000-mesh SiC sand paper, 15N pressure of a pressure head, 100r/min rotating speed of a clamp and 150r/min rotating speed of a turntable; polishing a surface to be measured of a sample for 5min by using 2000-mesh SiC sand paper, 5N pressure of a pressure head, 60r/min rotating speed of a clamp and 150r/min rotating speed of a turntable (the clamp turntable rotates in the same direction); and (3) adopting an automatic polishing machine, fixing the surface to be tested on a polishing clamp with the surface to be tested facing downwards, adopting velvet polishing cloth, spraying alumina polishing solution with the particle size of 0.5 microns on the polishing cloth, polishing the surface to be tested of the sample for 5min at the speed of 50r/min of a rotating disc (the rotating disc of the clamp rotates in the opposite direction) with the rotating speed of 100r/min of the clamp under the pressure of 5N, wherein absolute ethyl alcohol is used as a lubricant, the dropping speed of the lubricant is 2ml/min, obtaining a microscopic analysis sample, and drying and storing.
Microscopic analysis samples of the ultra-high performance concrete prepared in example 1, comparative example 1 and comparative example 2 were observed under an optical microscope as shown in fig. 1, 4 and 7, respectively. As is apparent from FIG. 1, the surface of the microscopic analysis sample of the quartz sand ultra-high performance concrete prepared by the method of the invention is basically free from scratches, and the interfaces of each phase are clear. FIG. 4 shows that the gel region has obvious overpolishing condition by adopting the conventional method, so that interface defects of each phase are caused, and microscopic analysis is not facilitated; the polishing of fig. 7 was insufficient and scratches were too pronounced.
The surface roughness of the samples of the ultra-high performance concrete microscopic analysis of examples 1 to 4 and comparative examples 1 and 2 was measured, and the results are shown in table 1.
TABLE 1 surface roughness of ultra-high Performance concrete microscopic analysis samples of examples 1 to 4 and comparative examples 1 and 2
As is apparent from table 1, the roughness of the surface of the ultra-high performance concrete microscopic analysis sample prepared by the method embodiment of the invention is better than that of the surface of the ultra-high performance concrete microscopic analysis sample prepared by the traditional method of the control group; from the 3D contour photograph and the line contour photograph of the surface of the quartz sand ultra-high performance concrete microscopic analysis sample prepared by the method disclosed by the invention, the surface of the ultra-high performance concrete microscopic analysis sample prepared by the method disclosed by the invention has more excellent smoothness, and the problem of uneven interface between aggregate and gel is better solved.
FIG. 8 is a photograph of a 20 μm ruler under SEM secondary electrons after 1 month of preservation of a quartz sand aggregate ultra-high performance concrete microscopic analysis sample preparation of example 1 of the present invention; as can be seen from the graph, the interface of each phase of the sample is clear, and no obvious hydration and carbonization trace exists on the surface. FIG. 9 is a photograph of a scale of 50 μm under SEM secondary electrons after 1 month of preservation of a sample for microscopic analysis of ultra-high performance concrete of quartz sand aggregate of comparative example 2, the surface of the sample is obviously attached with a plurality of square granular substances, covering the original surface structure of the sample. The comparison of the two is obvious, and the preservation mode adopted by the invention can prevent the surface to be tested from hydration and carbonization with air, and the test sample can be tested after long-term preservation.
Fig. 10 is a graph of the corundum aggregate ultra-high performance concrete (a) of the embodiment 5 after the hydration is terminated in the 6-hour age, from which it can be seen that the early ultra-high performance concrete has lower strength and is difficult to maintain the integrity of the structure, so that in order to perform early structure and early microscopic performance research, after the hydration is terminated, the impregnated mosaic is performed, and polishing is performed, so that the complete structure is obtained, as shown in fig. 10 (b), and the guarantee is provided for the subsequent accurate microscopic structure and microscopic mechanics test analysis.
The above examples are presented for clarity of illustration only and are not limiting of the embodiments. Other variations or modifications of the above description will be apparent to those of ordinary skill in the art, and it is not necessary or exhaustive of all embodiments, and thus all obvious variations or modifications that come within the scope of the invention are desired to be protected.

Claims (10)

1. The preparation method of the ultra-high performance concrete microscopic analysis sample is characterized by comprising the following steps of:
1) Cutting: cutting the ultra-high performance concrete test block to be tested into blocks by using a precise diamond cutting machine, exposing a fresh surface to be tested, and obtaining a block to be tested;
2) Terminating hydration: soaking the block to be tested obtained in the step 1) in alcohol, taking out, soaking in fresh alcohol, repeating for 4-5 times, and vacuum drying;
3) Rough polishing: coarsely polishing the surface to be tested of the sample for 20-60 s until the surface to be tested is smooth at the speed of 100-150 r/min by using 1000-mesh SiC sand paper; coarsely polishing the surface to be measured at a speed of 100-150 r/min until the surface to be measured is parallel to the upper and lower surfaces as much as possible;
4) And (3) fine grinding: finely grinding the block to be tested after the rough grinding in the step 3), wherein SiC sand paper with 2000 meshes, 3000 meshes and 5000 meshes is sequentially used, and the surface to be tested of the sample is respectively ground for 2-5 min at the pressure of 5-10N and the speed of 100-150 r/min;
5) Polishing: polishing the block to be tested after the fine grinding in the step 4), wherein silk polishing cloth is adopted to polish the surface to be tested of the sample for 30-90 s at a pressure of 5-10N and a speed of 50-100 r/min;
6) And (5) cleaning and drying: and 5) cleaning the polished block to be tested in the step 5) by using absolute ethyl alcohol, drying to obtain an ultra-high performance concrete microscopic analysis sample, and preserving in vacuum.
2. The method according to claim 1, wherein in the step 1), the aggregate in the ultra-high performance concrete raw material is one or more of machine-made sand, quartz sand, river sand and silicon carbide.
3. The method according to claim 1, wherein in the step 2), the alcohol is absolute ethanol or isopropanol.
4. The method according to claim 1, wherein in the step 2), the soaking time of the block to be tested in alcohol is 3 to 5 hours.
5. The method according to claim 1, wherein in the steps 3) to 5), absolute ethyl alcohol is used as a lubricant.
6. The method according to claim 5, wherein the lubricant is added at a rate of 2 to 10mL/min.
7. The method according to claim 1, wherein in the step 4), the automatic polishing machine is used for fine polishing; in the step 5), an automatic polishing machine is adopted for polishing.
8. The method according to claim 1, wherein in the step 5), polishing liquid having a particle size of 0.05 to 0.5 μm is sprayed on the polishing cloth.
9. The method according to claim 1, wherein in the step 6), the block to be tested is placed in absolute ethyl alcohol with the surface to be tested facing upwards, the block to be tested is placed in an ultrasonic cleaner, the block to be tested is cleaned for 3-8 min by ultrasonic, the sample to be tested is taken out, and the sample is dried by inert air flow, so that the ultra-high performance concrete microscopic analysis sample is obtained.
10. The preparation method according to claim 1, wherein when the age of the ultra-high performance concrete to be tested is less than or equal to 12 hours, the preparation method further comprises the steps of dipping and embedding, specifically comprising: placing the block to be tested after hydration termination in the step 2) into a silica gel mold, enabling the surface to be tested of the sample to be in contact with the bottom surface of the silica gel test mold, pouring the liquid curing agent into the silica gel test mold until the top of the sample is submerged, and standing the silica gel test mold until the curing agent is completely cured; wherein the liquid curing agent is epoxy resin or acrylic, and the standing time is as follows: epoxy resin for 3-8 h and acrylic for 20-30 min.
CN202310943079.0A 2023-07-27 2023-07-27 Preparation method of microscopic analysis sample of ultra-high-performance concrete Pending CN117007395A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117740499A (en) * 2023-12-19 2024-03-22 华中科技大学 Visualization method for three-dimensional microstructure of fiber-concrete interface transition zone

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117740499A (en) * 2023-12-19 2024-03-22 华中科技大学 Visualization method for three-dimensional microstructure of fiber-concrete interface transition zone

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