CN110361247A - A kind of preparation method of sample for nano impress Study on Steel fiber cement-based material median surface transition region performance - Google Patents
A kind of preparation method of sample for nano impress Study on Steel fiber cement-based material median surface transition region performance Download PDFInfo
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- CN110361247A CN110361247A CN201910639323.8A CN201910639323A CN110361247A CN 110361247 A CN110361247 A CN 110361247A CN 201910639323 A CN201910639323 A CN 201910639323A CN 110361247 A CN110361247 A CN 110361247A
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- cement
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/04—Portland cements
-
- 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
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/40—Investigating hardness or rebound hardness
- G01N3/42—Investigating hardness or rebound hardness by performing impressions under a steady load by indentors, e.g. sphere, pyramid
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- Inorganic Chemistry (AREA)
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- Materials Engineering (AREA)
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- Organic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a kind of preparation method of sample for nano impress Study on Steel fiber cement-based material median surface transition region performance, including consider that the ratio of mud, steel fibre pour steel fiber feinforced cement base mortar specimen；Test block through standard curing in 28 days is cut；The small sample cut with epoxy sealing；It polished small sample surface, polished；To examine the flatness on small sample surface decide whether that nano indentation test can be carried out with atomic force microscope observation small sample surface topography.The invention patent technology provides a whole set of and is used to prepare the method using nano impress Study on Steel fiber cement-based material median surface transition region performance sample, is of great significance to the research of cement-based material median surface transition region performance.
Description
Technical field:
The present invention relates to concrete material fields, specifically, being a kind of fiber cement-based for nano impress Study on Steel
The preparation method of sample of material median surface transition region performance.
Background technique:
The interfacial transition zone of cement-based material is the weak link of cement-based material, intensity for cement-based material and resistance to
Long property has important influence.Since the porosity in the region is larger, compactness is lower, the power of cement-based material is directly affected
Learn performance and endurance quality.When mineral admixture, such as silicon powder, flyash is added, the interface of cement-based material can be effectively improved
The density of transition region.
It on the other hand, is the cracking resistance and fracture toughness that improve cement-based material, steel fibre is widely added to water
In cement-based material.But the addition of steel fibre can introduce new fiber-aggregate-basal body interface area, so that this region also becomes
The weak link of cement-based material.Thus, it is necessary to steel fibre-aggregate-basal body interface transition region is studied, with determination
The preferable dosage of steel fibre.
Currently, focusing primarily upon aggregate-basal body interface transition region to the research of cement-based material interfacial transition zone.To containing
The research of the cement-based material interfacial transition zone of steel fibre and addition mineral admixture is less；Simultaneously as micro-indentations test
Limitation, Nanoindentation are increasingly being used in the research to cement-based material interfacial transition zone.But to containing steel fibre and plus
Enter the cement-based material of mineral admixture, the flatness for the cement base specimen surface for how ensuring to prepare is using nano impress
Key of the technical research containing steel fibre and the cement-based material interfacial transition zone performance that mineral admixture is added.It is existing to use nanometer
Research of the indentation to cement-based material interfacial transition zone performance, it is most of not contain steel fibre.
Summary of the invention:
For these reasons, the present invention is intended to provide a kind of be used for nano impress Study on Steel fiber cement-based material median surface
The preparation method of sample of transition region performance.
To achieve the above object, the invention adopts the following technical scheme: a kind of study steel fiber feinforced cement for nano impress
The preparation method of sample of sill median surface transition region performance, step include:
Step 1: prepare cement, 0-4mm and 0-2mm sand, agstone, silicon powder, steel fibre, water-reducing agent and mixing water；
Wherein cement is ordinary portland cement；SiO in silicon powder2Content is greater than 90%；Lime content is in agstone
79.8%；The fineness modulus of 0-4mm and 0-2mm sand is respectively 2.37 and 1.51；Steel fibre be diameter 0.16mm, long 13mm it is straight
High-carbon steel fibre；Solid content is 15% in water-reducing agent.
Step 2: preparing the ratio of mud respectively and be 0.3 and 0.5 mortar, including contains only steel fibre mortar and silicon powder-containing steel fibre
Tie up mortar；
The step of preparing steel fibre mortar are as follows: cement-based material (cement, agstone and (or) silicon powder) and sand exist
It is mixed and stirred under low speed 1 minute；In subsequent 4 minutes, the mixing water and water-reducing agent of half is first added, divides small lot that steel is added fine
Dimension, high-speed stirred；Add the other half mixing water；Stop 1 minute, stirring surrounding attachment is scraped into standing 5 minutes；Then
Low speed mixes and stirs 1 minute again.
Step 3: 40 × 40 × 160mm (wide × high × long) cuboid is poured respectively, is conserved 28 days in 20 DEG C of water；Often
The mortar of one type pours 6 40 × 40 × 160mm (wide × high × long) cuboid, wherein three are used to be ready for receiving altogether
The small sample of rice indentation test.
Step 4: maintenance in 28 days terminates, among 40 × 40 × 160mm (wide × high × long) cuboid position cutting 15 ×
The small cubes of 15 × 15mm, to obtain the more uniform cement base sample of quality, with epoxy sealing (specific steps such as Fig. 1 institute
Show)；
Step 5: the drying small sample (as shown in Figure 2) obtained to step 4 carries out beating for nano indentation test front surface
Mill, polishing；
To different types of small sample, first uses 1000 mesh silicon carbide water-proof abrasive papers, ground using water as lubricant semi-automatic
It is roughly ground 20 minutes on grinding machine, then carries out fine grinding on full-automatic metallurgical polishing grinder.The polishing of different type small sample is thrown
Light stream journey, as shown in table 1-2.Ultrasonic cleaning is carried out after each sanding and polishing, and is observed using microscope, it is ensured that on
Level-one scratch has been eliminated.
Step 6: using atomic force microscope observation small sample surface topography, to examine the flatness on small sample surface, determines
Whether nano indentation test can be carried out.If flatness meets, nano indentation test can be carried out.
The polishing of table 1 water-cement ratio, 0.3 two kinds of steel fibre mortar small samples, polishing flow process
The polishing of table 2 water-cement ratio, 0.5 two kinds of steel fibre mortar small samples, polishing flow process
Detailed description of the invention:
Fig. 1 is prepared by sample of the present invention for nano impress Study on Steel fiber cement-based material median surface transition region performance
The cutting of method, preparation cement base sample block diagram
Fig. 2 is prepared by sample of the present invention for nano impress Study on Steel fiber cement-based material median surface transition region performance
Small sample schematic diagram that the is epoxy sealing of method, dry, preparing polishing, polishing.
Specific embodiment:
The present invention including the following steps:
Step 1: prepare prepare cement-based material raw material, including cement, 0-4mm and 0-2mm sand, agstone,
Silicon powder, steel fibre, water-reducing agent and mixing water；
To prepare cement-based material cement, 0-4mm and 0-2mm sand, agstone and silicon powder, need to carry out cement,
The measurement of the chemical component of agstone and silicon powder；To 0-4mm and 0-2mm sand, its grain composition need to be determined；
Step 2: it prepares water-cement ratio and is 0.3 mortar, including contain only steel fibre mortar and silicon powder-containing steel fibre mortar；Match
Water-cement ratio processed is 0.5 mortar, including contains only steel fibre mortar and silicon powder-containing steel fibre mortar；
Steel fibre mortar and silicon powder-containing steel fibre mortar are contained only to two kinds of water-cement ratios, pay attention to cement-based material (cement, stone
Limestone flour and (or) silicon powder) and sand answer first uniform mixing；When steel fibre is added, it should be noted that add steel fibre point small lot for several times
Enter, with guarantee steel fibre it is relatively uniform be dispersed in mortar mix；It, should be by container week after whole water-reducing agents and mixing water is added
The attachment enclosed sufficiently scrapes into mortar mix, to guarantee that source material mixture ratio does not change；
During the above mortar mixes and stirs, standing 5 minutes is to allow water-reducing agent to play one's part to the full.
Step 3: the mortar for being 0.3 and 0.5 with the water-cement ratio prepared pours the cuboid of 40 × 40 × 160mm respectively；
Demoulding after 24 hours；And it is conserved 28 days in 20 DEG C of water；
When the mortar for being 0.3 and 0.5 with the water-cement ratio of preparation pours the cuboid of 40 × 40 × 160mm, it should be noted that vibration
It smashes uniformly；Demoulding after test specimen 24 hours is then placed in 20 DEG C of water and conserves 28 days；
Step 4: after the cuboid of 40 × 40 × 160mm (wide × high × long) conserves 28 days in 20 DEG C of water, cutting is obtained
Small cubes two of 15 × 15 × 15mm (wide × high × long).15 × 15 × 15mm small sample is placed in cylindrical plastic box
In, inject prepared epoxy liquid (specific steps are as shown in Figure 1)；Plastic casing is cut after epoxy drying and moulding, polished,
The small sample (Fig. 2) of polishing；
The cuboid of 40 × 40 × 160mm (wide × high × long) after maintenance 28 days is cut along cuboid width direction
The 10mm of the outer surface of two sides obtains the cuboid of 20 × 40 × 160mm (wide × high × long)；Again along its short transverse, cut
The 10mm of the outer surface of two sides obtains 20 × 20 × 160mm (wide × high × long) cuboid；The 40mm among obtained cuboid
Section is respectively cut small cubes 3 of 15 × 15 × 15mm (wide × high × long), is marked in test specimen side to distinguish.
15 × 15 × 15mm small sample is respectively placed in cylindrical plastic box, prepared epoxy liquid is injected；It is dry to epoxy
Plastic casing is cut after molding, the small sample polished, polished (such as Fig. 2 shows).
Step 5: to small sample shown in Fig. 2, using corase grinding, fine grinding and the process of polishing make specimen surface reach into
The flatness of row nano indentation test.
First roughly ground on semi-automatic grinder 20 minutes using water as lubricant, using 1000 mesh silicon carbide water-proof abrasive papers；So
It polished, polished on full-automatic metallurgical polishing grinder afterwards.To two kinds of steel fibre small samples of 0.3 water-cement ratio, according to table 1
The step of carry out, parameter setting including used sanding and polishing material, lubricant and full-automatic metallurgical polishing grinder (packet
Include the time, the grasping force and revolving speed that each sample is received)；To two kinds of steel fibre small samples of 0.5 water-cement ratio, according to the step of table 2
It is rapid to carry out, parameter setting including used sanding and polishing material, lubricant and full-automatic metallurgical polishing grinder (including when
Between, each sample grasping force and revolving speed received).
Ultrasonic cleaning is carried out after each sanding and polishing, and uses micro- sem observation surface of test piece, to ensure upper level
Scratch has been eliminated.
Step 6: to the small sample after sanding and polishing, using its surface topography of atomic force microscope observation, to examine
Whether the flatness on small sample surface can carry out nano indentation test；If not satisfied, it is primary to repeat step 5；Again using original
Sub- force microscope is examined；If having not been met, which cancels.
To the small sample after sanding and polishing, using its surface topography of atomic force microscope observation, to examine small sample
Whether the flatness on surface can carry out nano indentation test；Steel fiber surface, cement base matrix in main measurement small sample
The flatness on surface and aggregate (stone) surface.
If not satisfied, it is primary to repeat step 5；It is examined again using atomic force microscope；If having not been met, which makees
It is useless.
Claims (1)
1. a kind of preparation method of sample for nano impress Study on Steel fiber cement-based material median surface transition region performance, special
Sign be the following steps are included:
Step 1: prepare to prepare the raw material of cement-based material, including cement, 0-4mm and 0-2mm sand, agstone, silicon
Powder, steel fibre, water-reducing agent and mixing water；
Cement is ordinary portland cement；SiO in silicon powder2Content is greater than 90%；Lime content is 79.8% in agstone；0-
The fineness modulus of 4mm and 0-2mm sand is respectively 2.37 and 1.51；Steel fibre is diameter 0.16mm, the straight high-carbon steel of long 13mm is fine
Dimension；Solid content is 15% in water-reducing agent；
To cement, 0-4mm and 0-2mm sand, agstone and the silicon powder for preparing cement-based material, cement, agstone are carried out
With the measurement of the chemical component of silicon powder；To 0-4mm and 0-2mm sand, its grain composition need to be determined；
Step 2: it prepares water-cement ratio and is 0.3 mortar, including contain only steel fibre mortar and silicon powder-containing steel fibre mortar；Prepare water
Glue is than the mortar for 0.5, including contains only steel fibre mortar and silicon powder-containing steel fibre mortar；
The step of preparing mortar is as follows: by cement-based material, i.e. cement, agstone and/or silicon powder and sand is mixed under the low speed
With 1 minute；In subsequent 4 minutes, the mixing water and water-reducing agent of half is first added, divides small lot that steel fibre, high-speed stirring is added
It mixes；Add the other half mixing water；Stop 1 minute, stirring surrounding attachment is scraped into standing 5 minutes；Then low speed mixes and stirs again
1 minute；
Steel fibre mortar and silicon powder-containing steel fibre mortar are contained only to two kinds of water-cement ratios, pay attention to cement-based material, i.e. cement, lime
Mountain flour and/or silicon powder and sand answer first uniform mixing；When steel fibre is added, it should be noted that steel fibre point small lot is added for several times,
With guarantee steel fibre it is relatively uniform be dispersed in mortar mix；It, should be by container surroundings after whole water-reducing agents and mixing water is added
Attachment sufficiently scrape into mortar mix, to guarantee that source material mixture ratio does not change；
During the above mortar mixes and stirs, standing 5 minutes is to allow water-reducing agent to play one's part to the full；
Step 3: the mortar for being 0.3 and 0.5 with the water-cement ratio prepared pours the cuboid of 40 × 40 × 160mm respectively；24 is small
When after demoulding；And it is conserved 28 days in 20 DEG C of water；
Step 4: after 40 × 40 × 160mm wide × height × length cuboid conserves 28 days in 20 DEG C of water, along cuboid width,
Short transverse cuts the 10mm of the outer surface of two sides respectively, obtains 20 × 20 × 160mm wide × height × length cuboid；?
40mm section among the cuboid arrived, is respectively cut 15 × 15 × 15mm wide × height × length small cubes two；By 15 × 15
× 15mm small sample is placed in cylindrical plastic box, injects prepared epoxy liquid；Plastics are cut after epoxy drying and moulding
Box, the small sample polished, polished；
Step 5: the small sample obtained to step 4 makes specimen surface reach progress using corase grinding, fine grinding and the process of polishing
The flatness of nano indentation test；
First roughly ground on semi-automatic grinder 20 minutes using water as lubricant, using 1000 mesh silicon carbide water-proof abrasive papers；Then exist
It polished, polished on full-automatic metallurgical polishing grinder；To two kinds of steel fibre small samples of 0.3 water-cement ratio, according to the step of table 1
It is rapid to carry out, the parameter setting including used sanding and polishing material, lubricant and full-automatic metallurgical polishing grinder, including when
Between, each sample grasping force and revolving speed received；To two kinds of steel fibre small samples of 0.5 water-cement ratio, according to the step of table 2 into
Row, the parameter setting including used sanding and polishing material, lubricant and full-automatic metallurgical polishing grinder, including the time,
The grasping force and revolving speed that each sample is received；
Ultrasonic cleaning is carried out after each sanding and polishing, and uses micro- sem observation surface of test piece, to ensure upper level scratch
It has been eliminated；
Step 6: to the small sample after sanding and polishing, using its surface topography of atomic force microscope observation, to examine lab scale
Whether the flatness on sample surface can carry out nano indentation test；Steel fiber surface, cement base base in main measurement small sample
The flatness in body surface face and aggregate surface；Here aggregate, that is, stone；If not satisfied, it is primary to repeat step 5；Atom is used again
Force microscope is examined；If having not been met, which cancels.
The polishing of table 1 water-cement ratio, 0.3 two kinds of steel fibre mortar small samples, polishing flow process
The polishing of table 2 water-cement ratio, 0.5 two kinds of steel fibre mortar small samples, polishing flow process
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Cited By (4)
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| CN111024465A (en) * | 2019-12-03 | 2020-04-17 | 柳州钢铁股份有限公司 | Preparation method of sample for static phase change test |
| CN111693736A (en) * | 2020-06-22 | 2020-09-22 | 湘潭大学 | Section sample of lithium ion battery electrode plate for atomic force microscope characterization and preparation method thereof |
| CN112082863A (en) * | 2020-09-11 | 2020-12-15 | 山东大学 | Method for testing microcosmic bonding strength and elastic modulus of transition zone of concrete interface |
| CN117629709A (en) * | 2023-11-30 | 2024-03-01 | 华中科技大学 | Method for continuously measuring indentation modulus of interface transition zone in concrete |
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