CN110161218A - Method that is a kind of while measuring cement slurry chemical shrinkage amount Yu apparent volume variable quantity - Google Patents
Method that is a kind of while measuring cement slurry chemical shrinkage amount Yu apparent volume variable quantity Download PDFInfo
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- CN110161218A CN110161218A CN201910366562.0A CN201910366562A CN110161218A CN 110161218 A CN110161218 A CN 110161218A CN 201910366562 A CN201910366562 A CN 201910366562A CN 110161218 A CN110161218 A CN 110161218A
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- 239000004568 cement Substances 0.000 title claims abstract description 113
- 239000002002 slurry Substances 0.000 title claims abstract description 73
- 239000000126 substance Substances 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000007788 liquid Substances 0.000 claims abstract description 26
- 238000003384 imaging method Methods 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims description 7
- 238000005481 NMR spectroscopy Methods 0.000 claims 1
- 230000005251 gamma ray Effects 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 5
- 238000003780 insertion Methods 0.000 abstract 1
- 230000037431 insertion Effects 0.000 abstract 1
- 238000005259 measurement Methods 0.000 description 4
- 230000008602 contraction Effects 0.000 description 3
- JGSARLDLIJGVTE-UHFFFAOYSA-N 3,3-dimethyl-7-oxo-6-[(2-phenylacetyl)amino]-4-thia-1-azabicyclo[3.2.0]heptane-2-carboxylic acid Chemical compound O=C1N2C(C(O)=O)C(C)(C)SC2C1NC(=O)CC1=CC=CC=C1 JGSARLDLIJGVTE-UHFFFAOYSA-N 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000005662 Paraffin oil Substances 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000013170 computed tomography imaging Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007571 dilatometry Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229940057995 liquid paraffin Drugs 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000003325 tomography Methods 0.000 description 1
- 238000013316 zoning Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/38—Concrete; Lime; Mortar; Gypsum; Bricks; Ceramics; Glass
- G01N33/383—Concrete or cement
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- Chemical & Material Sciences (AREA)
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- Medicinal Chemistry (AREA)
- Food Science & Technology (AREA)
- Ceramic Engineering (AREA)
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- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The invention discloses a kind of method for measuring cement slurry chemical shrinkage amount Yu apparent volume variable quantity simultaneously, specifically: first mix cement slurry, and then cement slurry is fitted into sample bottle, and blend rubber plug seals up bottleneck, then will be in buret insertion rubber plug；Add water into sample bottle by buret, until stopping adding water at the scale of water level amount of reach tube top end in buret, grease-like liquid is added dropwise in vector tube at this time, the liquid level initial reading of buret is recorded when cement sample carries out imaging for the first time；Multiple time points are chosen to the multiple three-dimensional imaging of sample progress, and record the buret liquid level readings of sample simultaneously；Chemical shrinkage value is obtained from collected liquid level readings data；Digital volume related (DVC) is carried out to the 3-D image of different time acquisition to calculate, and obtains sample in three principal strain values of different periods, and further find out the variation of cement slurry apparent volume；Finally compare the variation connection of chemical shrinkage value and apparent volume.
Description
Technical field
The present invention relates to a kind of methods for measuring cement slurry chemical shrinkage amount Yu apparent volume variable quantity simultaneously.
Background technique
As efficient additive, low water binder ratio, big mineral admixture and high grade of cement are increasingly becoming configuration concrete
The deformation properties of mainstream technology, modern concrete early stage are also changed, and chemical shrinkage and the self-constriction being affected by it are total
Proportion is increasing in contraction distortion, it has also become and concrete generates the main reason for contraction distortion crackle, so, study water
The chemical shrinkage of cement-based material is extremely important.
Chemical shrinkage refers in cement hydration process, the absolute body of the absolute volume of hydrated product than cement before aquation and water
The phenomenon that the sum of product is reduced.The volume of reduction is largely changed into the hole of cement slurry or inside concrete, few part quilt
Occupied by self-constriction.Currently, the method for measurement chemical shrinkage includes plavini, gravimetric method, pyknometry.Wherein, weight
Method reflects chemical shrinkage according to the buoyancy variation of detection test specimen, although computer-automatic collection data, device can be used in it
Complex, use is not convenient enough.And pycnometric determination normal direction sample water injecting compensation cement slurry leads to because of the volume of aquation reduction
Specific gravity variation reflection chemical shrinkage value is crossed, notable defect existing for this method is that test sample size and experimental temperature influence seriously,
Error is larger, and plavini directly obtains the volume change of slurry, accuracy and economy by detection liquid level
It has obtained generally approving, thus has been most widely used.Plavini is carried out generally according to measurement standard ASTM C1608.Mixing cement
Continue after slurry injection beaker to beaker plus water is to completely, the rubber stopper for being inserted with capillary is covered into beaker, drop is suitable on the capillary water surface
Amount paraffin oil is to reduce moisture evaporation, and 23 DEG C of water bath with thermostatic control maintenances, 1h starts to read after cement slurry mixes and stirs, from liquid level decline pair
The volume change answered obtains chemical shrinkage value.
It is well known that the deformation inside cement slurry is extremely complex, in addition to chemical shrinkage, there are also temperature deformation, crystallization pressures
Expansion, entringite expansion etc., to influence the apparent volume of cement slurry, i.e., both there is represent absolute volume for cement slurry
Reduced chemical shrinkage, while there is the variation of itself apparent volume again.However the method for above-mentioned three kinds of measurements chemical shrinkage obtains
To be all cement slurry absolute volume variation, can not obtain cement slurry apparent volume variation.Due to cement slurry
The problems such as apparent volume variation is small, and dilatometry is difficult, traditional method can only reflect single chemical shrinkage, cannot but quantify
Ground, which provides, is occurring the apparent volume deformation that the cement slurry of chemical shrinkage has, and therefore, there is an urgent need to a kind of methods to go together
When measurement cement slurry chemical shrinkage amount and apparent volume changing value.
Summary of the invention
Goal of the invention: cement slurry chemical shrinkage amount is measured simultaneously technical problem to be solved by the invention is to provide a kind of
With the method for apparent volume variable quantity, this method can measure cement slurry while measuring cement slurry chemical shrinkage amount
Apparent volume variable quantity can obtain apparent volume variable quantity by analyzing the relationship of apparent volume change and chemical shrinkage amount
Influence to chemical shrinkage amount, to obtain more true chemical shrinkage amount, therefore the method for the present invention can be subsequent analysis
Data supporting is provided.
Method that is a kind of while measuring cement slurry chemical shrinkage amount Yu apparent volume variable quantity, specifically includes following step
It is rapid:
It step 1, will be V than volumecCement powder with than volume be VdWater be mixed to be formed the ratio of mud be W cement
Slurry seals with rubber stopper bottleneck after being packed into the cement slurry of mass M into sample bottle, and buret is passed through rubber stopper and protrudes into sample
In mouth bottle；
Step 2, add water into sample bottle by buret, until stopping adding water at the scale of water level amount of reach tube top end, at this time
Grease-like liquid is added dropwise in vector tube again, the liquid level initial reading of buret, note are recorded when cement sample be imaged for the first time
For V0；
Step 3, multiple time point t are chosen, three-dimensional imaging is carried out to cement sample, obtain different time points t cement sample
3 d image data, while the buret liquid level readings of corresponding time point cement sample are recorded, it is denoted as Vt, sample is calculated with public formula (I)
Chemical shrinkage amount CS of the product in t momentt；
In formula, CStFor the chemical shrinkage of cement sample t moment；VtFor the buret liquid level readings of cement sample t moment, mL；
V0For the liquid level initial reading of buret, mL；W is the ratio of mud of cement slurry；M is the quality of cement slurry in sample bottle, g；VdFor
The ratio volume of water, cm3·g-1；VcFor the ratio volume of cement powder, cm3·g-1；
Step 4, DVC calculating is carried out to the cement sample multiple groups 3 d image data that step 3 obtains, DVC includes existing
Using the DVC of various algorithms, to obtain the mean strain value in three directions of cement sample, it is denoted as ex, ey, ez, cement slurry
Sample apparent volume strain value is obtained with public formula (II)；
Ev=ex+ey+ez (II)
In formula, ev is cement slurry bulk strain value；Ex is the mean strain on cement slurry horizontal plane along the x axis
Value；Ey is the mean strain value on cement slurry horizontal plane along the y axis；Ez is in cement slurry vertical direction along Z axis direction
Mean strain value.
The utility model has the advantages that the method for the present invention can be simultaneously compared with the conventional method that can only measure single chemical shrinkage amount
The chemical shrinkage amount and apparent volume variable quantity of cement slurry are measured and distinguish, it can be by analyzing apparent volume change and chemistry
The relationship of shrinkage obtains influence of the apparent volume variable quantity to chemical shrinkage amount, to obtain more true chemical shrinkage
Amount, so that new thinking is provided for research early stage cement deformation, to various cement of the research including expansion compensation cement
Early deformation is provided convenience.
Detailed description of the invention
Fig. 1 is Experimental equipment of the invention；
Fig. 2 is the cement slurry sample CT slice of data that the present invention is obtained by x-ray tomography method；
Fig. 3 is the cement sample chemical shrinkage amount time history plot that the present invention obtains；
Fig. 4 is the corresponding relationship that the present invention calculates that the cement slurry swell increment obtained is changed over time by DVC；
Fig. 5 is the present invention in different time sections, the relationship of cement sample chemical shrinkage amount and cement slurry swell increment.
Specific embodiment
Below in conjunction with drawings and examples, technical scheme is described further, but claimed
Range be not limited thereto.
The method that the present invention measures cement slurry chemical shrinkage amount Yu apparent volume variable quantity simultaneously, first mix cement slurry
Then cement slurry is fitted into sample bottle by body, blend rubber plug seals up bottleneck, then buret is inserted into rubber plug；Throughput
Pipe adds water into sample bottle, until stopping adding water at the scale of water level amount of reach tube top end in buret, grease is added dropwise in vector tube at this time
Class I liquid I records the liquid level initial reading of buret when cement sample be imaged for the first time；Multiple time points are chosen to sample
Multiple three-dimensional imaging is carried out, and records the buret liquid level readings of sample simultaneously；Chemistry is obtained from collected liquid level readings data
Shrinkage value；Digital volume related (DVC) is carried out to the 3-D image of different time acquisition to calculate, and obtains sample in different periods
Three principal strain values, and further find out the variation of cement slurry apparent volume；Finally compare chemical shrinkage value and apparent volume
Variation connection.
The method of the present invention body includes the following steps:
Step 1, it mixes and stirs cement powder and water to form cement slurry, cement powder is Jiangnan little Ye field PII52.5 grade, ratio
Volume Vc=0.311cm3·g-1, water than volume Vd=1cm3·g-1, the ratio of mud of cement slurry is 0.5；To medical cillin bottle
The middle cement slurry for being packed into quality 2g, blend rubber plug seal up the bottleneck of cillin bottle, then by capacity are 0.9mL, minimum scale
It is inserted into rubber stopper for the buret of 0.001mL, as shown in Figure 1；
Step 2, with syringe by adding water in buret westwards woods bottle, until reaching at buret top scale (i.e. corresponding
Scale is at the position 0mL), stop adding water, instill a drop of liquid paraffin in vector tube at this time and be sealed, is carried out to cement sample
(using corresponding buret liquid level readings after sample formation 1.3 hours as initial reading, i.e., corresponding scale when first time CT is imaged
The liquid level initial reading that buret is recorded for 0.042mL), is denoted as V0；
Step 3, it chooses suitable scan position and time point t carries out three-dimensional X-CT imaging, to obtain 3-D image number
According to；Imaging device used is Zeiss Xradia 510X ray microscope, and scanning center position is hung down from cement sample/water termination
Directly distance A is 3.3mm, and sweep time t is that cement sample forms 1.3 hours, 6.3 hours, 13 hours, 25 hours and 52 hours,
X-CT sweep parameter are as follows: scanning 80 kilovolts of crest voltage, 7 watts of power, every the projection exposure time 1.2 seconds, 13 microns of resolution ratio,
Scanning obtains two-dimensional ct slice map (as shown in Figure 2) every time；In addition, being recorded in the liquid level readings V of t moment buret simultaneouslyt, respectively
It is 0.042,0.043,0.0595,0.072 and 0.083, the chemical shrinkage amount CS of cement sample is found out using calculation formula (I)t；
In formula, CStFor the chemical shrinkage of cement sample t moment；VtFor the buret liquid level readings of cement sample t moment, mL；
V0For the liquid level initial reading of buret, mL；W is the ratio of mud of cement slurry；M is the quality of cement slurry in sample bottle, g；VdFor
The ratio volume of water, cm3·g-1；VcFor the ratio volume of cement powder, cm3·g-1；Finally obtain what chemical shrinkage amount changed over time
Curve graph, as shown in Figure 3；
Step 4, the 3 d image data of the cement sample obtained to step 3 carries out DVC calculating, obtains slurry apparent volume
Deflection: the zoning of selection be 400 × 400 × 500 voxels, with 1.3 hours and 6.3 hours one group, 6.3 hours with
13 hours one group, 13 hours and 25 hours one group, 25 hours and 52 hours one group of carry out DVC, which are calculated, obtains each group cement slurry
Three principal strain values, and find out with calculation formula (II) the apparent volume deflection of sample in different time region；To obtain
The corresponding relationship of apparent volume deformation values and time, as shown in Figure 4.
Every group of period corresponds to the mean strain value in three directions of cement sample, is ex, ey, ez, therefore this group of time
Section cement slurry apparent volume strain value is obtained with public formula (II)；
Ev=ex+ey+ez (II)
In formula, ev is cement slurry bulk strain value；Ex is the mean strain value of cement slurry along the x axis；Ey is water
The mean strain value of slurry body along the y axis；Ez is mean strain value of the cement slurry along Z-direction.
The bulk strain for the cement slurry sample that the chemical shrinkage amount for the cement sample that step 3 obtains and step 4 are obtained
Data are depicted as curve graph under the same coordinate, as shown in figure 5, obtaining the pass between chemical shrinkage amount and bulk strain amount
System.
From the experimental data of Fig. 3 it is found that chemical shrinkage rate several hours after cement slurry molding are smaller, then to water
Changing chemical shrinkage within one day has apparent acceleration.It has crossed after one day, chemical shrinkage rate, which starts again at, to be slowed down.In conjunction with change
It learns to shrink and obtains Fig. 5 with apparent volume deformation, characterize the corresponding relationship between chemical shrinkage and apparent volume for the first time, find
The ratio of mud be 0.5 cement slurry: the chemical shrinkage gentle phase before forming 6.3h, the apparent volume of cement slurry have compared with
Big dilatancy almost accounts for the one third of chemical contraction of cement；During the accelerated period of aquation, i.e. 6.3h to 25h, water
The apparent volume of slurry body no longer shows to expand, but shrinks, and shrinkage is much smaller for chemical shrinkage amount；
After chemical shrinkage is again introduced into the gentle phase, i.e. after 25h, the apparent volume of cement slurry have again a small amount of expansion and by
It gradually tends towards stability, but still has very big chemical shrinkage at this time.
Claims (4)
1. a kind of method for measuring cement slurry chemical shrinkage amount Yu apparent volume variable quantity simultaneously, which is characterized in that specific packet
Include following steps:
It step 1, will be V than volumecCement powder with than volume be VdWater be mixed to be formed the ratio of mud be W cement slurry,
Bottleneck is sealed with rubber stopper after being packed into the cement slurry of mass M into sample bottle, buret is passed through into rubber stopper and stretches sample inlet port bottle
In；
Step 2, by buret into sample bottle plus water, until stop at the scale of water level amount of reach tube top end plus water, at this time again to
Grease-like liquid is added dropwise in buret, the liquid level initial reading of buret is recorded when cement sample be imaged for the first time, is denoted as V0；
Step 3, multiple time point t are chosen, three-dimensional imaging is carried out to cement sample, obtain the three-dimensional of different time points t cement sample
Image data, while the buret liquid level readings of corresponding time point cement sample are recorded, it is denoted as Vt, sample is calculated in t with public formula (I)
The chemical shrinkage amount CS at momentt；
In formula, CStFor the chemical shrinkage of cement sample t moment；VtFor the buret liquid level readings of cement sample t moment, mL；V0For
The liquid level initial reading of buret, mL；W is the ratio of mud of cement slurry；M is the quality of cement slurry in sample bottle, g；VdFor water
Ratio volume, cm3·g-1；VcFor the ratio volume of cement powder, cm3·g-1；
Step 4, DVC calculating is carried out to the cement sample multiple groups 3 d image data that step 3 obtains, to obtain cement sample three
The mean strain value in a direction, is denoted as ex, ey, ez, and cement slurry sample apparent volume strain value is obtained with public formula (II)；
Ev=ex+ey+ez (II)
In formula, ev is cement slurry bulk strain value；Ex is the mean strain value of cement slurry along the x axis；Ey is cement slurry
The mean strain value of body along the y axis；Ez is mean strain value of the cement slurry along Z-direction.
2. method that is according to claim 1 while measuring cement slurry chemical shrinkage amount Yu apparent volume variable quantity,
Be characterized in that: in step 2, grease-like liquid is atoleine.
3. method that is according to claim 1 while measuring cement slurry chemical shrinkage amount Yu apparent volume variable quantity,
Be characterized in that: in step 3,3 d image data refers to using X-ray, gamma ray, nuclear magnetic resonance, neutron imaging or electronic display
The 3 d image data that micro mirror obtains.
4. method that is according to claim 1 while measuring cement slurry chemical shrinkage amount Yu apparent volume variable quantity,
Be characterized in that: in step 3, when carrying out three-dimensional imaging, scanning center position is located at the lower section of cement slurry and water termination.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110967353A (en) * | 2019-12-09 | 2020-04-07 | 东南大学 | Method for measuring water absorption and release curve of SAP in cement paste based on ray imaging |
| CN111323567A (en) * | 2020-03-16 | 2020-06-23 | 同济大学 | Cement paste chemical shrinkage testing device and application thereof |
| CN113341113A (en) * | 2021-04-30 | 2021-09-03 | 东南大学 | Method for matching corresponding drying shrinkage under humidity gradient in cement-based material |
| CN114660273A (en) * | 2022-02-25 | 2022-06-24 | 襄阳市正实建设工程质量检测有限公司 | Cement quality detection method and cement quality detection system |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110967353A (en) * | 2019-12-09 | 2020-04-07 | 东南大学 | Method for measuring water absorption and release curve of SAP in cement paste based on ray imaging |
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| CN113341113A (en) * | 2021-04-30 | 2021-09-03 | 东南大学 | Method for matching corresponding drying shrinkage under humidity gradient in cement-based material |
| CN113341113B (en) * | 2021-04-30 | 2023-09-19 | 东南大学 | Method for matching corresponding drying shrinkage under humidity gradient in cement-based material |
| CN114660273A (en) * | 2022-02-25 | 2022-06-24 | 襄阳市正实建设工程质量检测有限公司 | Cement quality detection method and cement quality detection system |
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Application publication date: 20190823 |