CN103278423B - Quantitative characterization method for calcium carbonate space distribution in carbonized cement-based material - Google Patents

Quantitative characterization method for calcium carbonate space distribution in carbonized cement-based material Download PDF

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CN103278423B
CN103278423B CN201310189839.XA CN201310189839A CN103278423B CN 103278423 B CN103278423 B CN 103278423B CN 201310189839 A CN201310189839 A CN 201310189839A CN 103278423 B CN103278423 B CN 103278423B
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calcium carbonate
carbonization
cement
based material
compressing tablet
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CN103278423A (en
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万克树
徐琼
王宇东
潘钢华
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Southeast University
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Abstract

The invention discloses a quantitative characterization method for space distribution of calcium carbonate volume content in a carbonized cement-based material. The quantitative characterization method disclosed by the invention is used for calculating the volume content of calcium carbonate through gray level difference of a sample before and after carbonization and based on three-dimensional X ray tomography gray level data. The nondestructive characteristic and three-dimensional perspective characteristic of X ray tomography technology are adopted to realize the quantitative characterization of calcium carbonate space distribution in the partially carbonized cement-based material on the premise of not damaging the sample, and the method also can be used for figuring out the evolution process of calcium carbonate content with carbonization time in the same sample.

Description

The quantitatively characterizing method of calcium carbonate space distribution in a kind of carbonization cement-based material
Technical field
The present invention relates to the quantitatively characterizing method of calcium carbonate space distribution in a kind of carbonization cement-based material, belong to cement-based material permanance category, be mainly used in various cement-based material carbonization permanance investigation and application.
Background technology
Cement concrete is widely used in productive life, but performance can constantly deterioration in process under arms for this kind of material, so a study hotspot in the cement-based material permanance outer civil engineering material field that is Present Domestic, to human kind sustainable development and the development of the national economy significant.Carbonization is a kind of typical permanance form, causes hole solution ph to reduce, cause rebar passivation film to disappear because of carbonization, steel bar corrosion thus cause materials and structures to lose efficacy.Carbonization becomes calcium carbonate by the calcium hydroxide in cement-based material and hydrated calcium silicate gel part, so calcium carbonate is characterized in cement-based material carbonization research extremely important.
Conventional cement-based material carbonization characterizing method has: phenolphthalein indicator method; X-ray diffraction method, thermal analysis system; Electron probe method.Phenolphthalein indicator method reflects carbonation depth indirectly by means of pH value, but its degree of depth measured is inaccurate and influenced factor is many.X-ray diffraction method, thermal analysis system can obtain the assembly average of calcium carbonate and calcium hydroxide in analyzed powdered sample, but cannot provide the space distribution of carbonization.Although electron probe can obtain carbon distribution, exists quantitatively inaccurate to low atomic number carbon, sample preparation complicated and easily lesioned sample, measure problems such as being limited to locally, time-consuming is long, expense is high.All said methods are all damage analysis, cannot follow the tracks of the different carbonizing degree of a sample.
Tomography is a kind of computing method carrying out inverting physical model from observation data, will use complicated mathematical computations, because this conversion can only adopt computing machine, so be commonly referred to as computed tomography in inversion.X-ray tomography utilizes X ray to penetrate various material and after being partially absorbed exactly, at the transmitted intensity signal that detecting device obtains, calculates layer image carrying out process through computing machine to data.X-ray tomography has harmless observation, the advantage of three-dimensional perspective, so there is bright application prospect in material three-dimensional structural characterization field.
Disclosed patent CN201210017713.X provides a kind of method utilizing three-dimensional carbonation depth in x-ray tomography lossless detection cement-based material recently.Though the method can provide carbonation depth, the quantitative distribution of calcium carbonate cannot be provided.Carbonization is a progressive process, and it is also gradient distribution that the composition that it causes develops, and the quantity space distribution of calcium carbonate is all extremely important to carbonization study mechanism, Carbonation Model checking.
Summary of the invention
For the problem of existing quantitative test cement-based material carbonization difficulty, the invention provides the quantitatively characterizing method of calcium carbonate space distribution in a kind of carbonization cement-based material, can the three-dimensional spatial distribution of calcium carbonate that causes because of carbonization of quantitatively characterizing partially carbonized cement-based material inside.
Technical scheme of the present invention is:
A quantitatively characterizing method for calcium carbonate space distribution in carbonization cement-based material, the half-tone information obtained with x-ray tomography calculates the amount of calcium carbonate, comprises the following steps:
Step 1: get a forming and the cement-based material in maintenance certain length of time, drying obtains non-carbonized samples in an oven;
Step 2: setting tomography test condition, carries out first time x-ray tomography test to the non-carbonized samples that step 1 obtains, obtains the three-dimensional tomographic image data G of non-carbonized samples 0(x, y, z);
Step 3: the face not needing carbonization with melt paraffin sealing, puts into carbonization case, controls Carbonization Conditions, carry out accelerated carbonation;
Step 4: after carbonization certain hour, takes out accelerated carbonation sample, under the tomography test condition identical with step 2, carries out the test of second time x-ray tomography, obtains the three-dimensional tomographic image data G of accelerated carbonation sample 1(x, y, z);
Step 5: the accelerated carbonation sample carrying out the test of second time x-ray tomography is put into carbonization case again, with the same Carbonization Conditions of step 3 under again after carbonization certain hour, take out accelerated carbonation sample, under the tomography test condition identical with step 2, carry out third time x-ray tomography test, obtain the three-dimensional tomographic image data G of secondary accelerated carbonation sample 2(x, y, z);
Step 6: use G 0(x, y, z) is respectively to G 1(x, y, z) and G 2(x, y, z) carries out rigid registration, and the data after registration are with
Step 7: get calcium hydroxide and calcium carbonate powder crystal, is pressed into calcium hydroxide compressing tablet and the calcium carbonate compressing tablet of regular shape, is respectively ρ by the apparent density that weight method obtains described calcium hydroxide compressing tablet and calcium carbonate compressing tablet in conjunction with measurement volumes method with sheeter cH-is apparentand ρ caCO3-is apparent, then under the tomography test condition identical with step 2, x-ray tomography test is carried out to calcium hydroxide compressing tablet and calcium carbonate compressing tablet, obtains calcium hydroxide compressing tablet and the calcium carbonate compressing tablet three-dimensional tomographic image data G in different spatial cH-is apparent(x, y, z) and G caCO3-is apparent(x, y, z), gets the mean value of its different spatial three-dimensional tomographic image data respectively with combining hydrogen oxidation calcium solid density ρ cHwith calcium carbonate solid density ρ caCO3, the gray-scale value of calcium hydroxide and calcium carbonate is calculated respectively with following formula: with
Step 8: utilize following formulae discovery to obtain the three-dimensional spatial distribution of calcium carbonate volume content after different carbonization time:
f CaCO 3 1 ( x , y , z ) = G 1 reg ( x , y , z ) - G 0 ( x , y , z ) G CaCO 3 - ( 1 - 38 369 ) G CH
f CaCO 3 2 ( x , y , z ) = G 2 reg ( x , y , z ) - G 0 ( x , y , z ) G CaCO 3 - ( 1 - 38 369 ) G CH .
Further, cement-based material described in step 1 comprises clean slurry, mortar or concrete.
Further, Carbonization Conditions described in step 3 is carbon dioxide concentration expressed in percentage by volume is 10%-100%, and other composition can be the inert gas such as air or nitrogen, and relative humidity is 60%-80%, and temperature is 20-60 DEG C.
Further, x-ray tomography wherein adopts medical, industrial, micro-or nanometer x-ray tomography equipment.
Beneficial effect of the present invention:
The present invention can calculate from the half-tone information difference of the x-ray tomography data of cement-based material sample before and after carbonization the calcium carbonate content caused because of carbonization, by means of the feature of its nondestructive analysis and 3-D view, can the quantitative three-dimensional spatial distribution of calcium carbonate that causes because of carbonization of nondestructive characterisation (NDC) partially carbonized cement-based material inside, carbonization process and degree can more adequately be described.Relative to damaging analysis, the present invention can nondestructively follow the tracks of the different carbonizing degree of a sample, the spatial and temporal distributions of research calcium carbonate, thus studies carbonization mechanism further, setting up suitable Carbonation Model, is finally carbonization permanance and the life prediction service thereof of cement based structured material.
Accompanying drawing explanation
Fig. 1 is that cement slurry sample in embodiment 1 is at the exemplary two dimensional faultage image of carbonization after 14 days.
Fig. 2 be in the carbonization 14 days cement slurry samples in embodiment 1 calcium carbonate volume content along the one dimension distribution in carbonization direction and the contrast of calcium carbonate content that obtains with thermogravimetry (TG) measurement thereof.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention done and further explain.
Embodiment 1:
A quantitatively characterizing method for calcium carbonate space distribution in carbonization cement-based material, the half-tone information obtained with x-ray tomography calculates the amount of calcium carbonate, comprises the following steps:
Step 1: prepare with Portland cement the cement paste sample that water cement ratio is 0.53, sample size is 40mm × 40mm × 100mm, standard curing 28 days, then in the baking oven of 50 DEG C dry 48 hours;
Step 2: setting tomography test condition, accelerating potential 200kV, the electric current 0.3mA of setting x-ray tomography equipment, enlargement factor 3.3 times, first time x-ray tomography test is carried out to the sample obtained in step 1, obtains the three-dimensional tomographic image data G of non-carbonized samples 0(x, y, z);
Step 3: seal the face that four do not need carbonization with melt paraffin, only stays the face of two relative 40mm × 100mm, puts into carbonization case and carry out one dimension carbonization, control Carbonization Conditions: carbon dioxide concentration expressed in percentage by volume is 20%, relative humidity is 70 ± 5%, and temperature is 20 ± 2 DEG C, carries out accelerated carbonation;
Step 4: in carbonization after 14 days, takes out accelerated carbonation sample, under the tomography test condition identical with step 2, carries out the test of second time x-ray tomography, obtains the three-dimensional tomographic image data G of accelerated carbonation sample 1(x, y, z);
Step 5: the accelerated carbonation sample carrying out second time x-ray tomography is put into carbonization case again, carbonization 14 days again under the Carbonization Conditions identical with step 3, take out accelerated carbonation sample, under the tomography test condition identical with step 2, carry out third time x-ray tomography test, obtain the three-dimensional tomographic image data G of secondary accelerated carbonation sample 2(x, y, z);
Step 6: use G 0(x, y, z) is to G 1(x, y, z) and G 2(x, y, z) carries out rigid registration, and the data after registration are with
Step 7: get calcium hydroxide and calcium carbonate powder crystal, is pressed into calcium hydroxide compressing tablet and the calcium carbonate compressing tablet of regular shape, is respectively ρ by the apparent density that weight method obtains described calcium hydroxide compressing tablet and calcium carbonate compressing tablet in conjunction with measurement volumes method with sheeter cH-is apparentand ρ caCO3-is apparent, then under the tomography test condition identical with step 2, x-ray tomography test is carried out to calcium hydroxide compressing tablet and calcium carbonate compressing tablet, obtains calcium hydroxide compressing tablet and the calcium carbonate compressing tablet three-dimensional tomographic image data G in different spatial cH-is apparent(x, y, z) and G caCO3-is apparent(x, y, z), gets the mean value of its different spatial three-dimensional tomographic image data respectively with combining hydrogen oxidation calcium solid density ρ cHwith calcium carbonate solid density ρ caCO3, the gray-scale value of calcium hydroxide and calcium carbonate is calculated respectively with following formula: with
Step 8: utilize following formulae discovery to obtain the three-dimensional spatial distribution of calcium carbonate after different carbonization time:
f CaCO 3 1 ( x , y , z ) = G 1 reg ( x , y , z ) - G 0 ( x , y , z ) G CaCO 3 - ( 1 - 38 369 ) G CH
f CaCO 3 2 ( x , y , z ) = G 2 reg ( x , y , z ) - G 0 ( x , y , z ) G CaCO 3 - ( 1 - 38 369 ) G CH .
Embodiment 2
The present embodiment place different with embodiment 1 is, cement-based material is sand-cement slurry, dry in the baking oven of 60 DEG C, Carbonization Conditions is carbon dioxide concentration expressed in percentage by volume is 10%, relative humidity is 60 ± 5%, temperature is 40 ± 2 DEG C, and other concrete steps are identical with embodiment 1.
Embodiment 3
The present embodiment place different with embodiment 1 is, cement-based material is cement concrete, and Carbonization Conditions is carbon dioxide concentration expressed in percentage by volume is 100%, relative humidity is 80 ± 5%, temperature is 60 ± 2 DEG C, and other concrete steps are identical with embodiment 1.
Fig. 1 be in embodiment 1 grout sample at the exemplary two dimensional faultage image of carbonization after 14 days, Fig. 2 be in the carbonization 14 days cement slurry samples in embodiment 1 calcium carbonate volume content along the one dimension distribution in carbonization direction and the contrast of calcium carbonate content that obtains with thermogravimetry (TG) measurement thereof.In order to contrast verification the method, distance carbonization face 0-3mm is measured respectively with thermogravimetry (TG) (TGA), 4-6mm, 8-12mm, with the average external volume content of calcium carbonate in 13-17mm sample, the result average by the inventive method is also shown in Fig. 2, and the average result that therefrom visible two kinds of methods obtain has good anastomose property, thus demonstrates the inventive method.Advantage of the present invention is to obtain space three-dimensional space distribution more accurately.
The above is only one of embodiments of the invention, therefore all equivalences done according to structure, feature and the principle described in the present patent application scope change or modify, and are included within the scope of the present patent application.

Claims (4)

1. the quantitatively characterizing method of calcium carbonate space distribution in carbonization cement-based material, is characterized in that, the half-tone information obtained with x-ray tomography calculates the amount of calcium carbonate, comprises the following steps:
Step 1: get a forming and the cement-based material in maintenance certain length of time, drying obtains non-carbonized samples;
Step 2: setting tomography test condition, carries out first time x-ray tomography test to the non-carbonized samples that step 1 obtains, obtains the three-dimensional tomographic image data G of non-carbonized samples 0(x, y, z);
Step 3: the face not needing carbonization with melt paraffin sealing, puts into carbonization case, controls Carbonization Conditions, carry out accelerated carbonation;
Step 4: after carbonization certain hour, takes out accelerated carbonation sample, under the tomography test condition identical with step 2, carries out the test of second time x-ray tomography, obtains the three-dimensional tomographic image data G of accelerated carbonation sample 1(x, y, z);
Step 5: the accelerated carbonation sample carrying out the test of second time x-ray tomography is put into carbonization case again, with the same Carbonization Conditions of step 3 under again after carbonization certain hour, take out accelerated carbonation sample, under the tomography test condition identical with step 2, carry out third time x-ray tomography test, obtain the three-dimensional tomographic image data G of secondary accelerated carbonation sample 2(x, y, z);
Step 6: use G 0(x, y, z) is respectively to G 1(x, y, z) and G 2(x, y, z) carries out rigid registration, and the data after registration are with
Step 7: get calcium hydroxide and calcium carbonate powder crystal, is pressed into calcium hydroxide compressing tablet and the calcium carbonate compressing tablet of regular shape, is respectively ρ by the apparent density that weight method obtains described calcium hydroxide compressing tablet and calcium carbonate compressing tablet in conjunction with measurement volumes method with sheeter cH-is apparentand ρ caCO3-is apparent, then under the tomography test condition identical with step 2, x-ray tomography test is carried out to calcium hydroxide compressing tablet and calcium carbonate compressing tablet, obtains calcium hydroxide compressing tablet and the calcium carbonate compressing tablet three-dimensional tomographic image data G in different spatial cH-is apparent(x, y, z) and G caCO3-is apparent(x, y, z), gets the mean value of its different spatial three-dimensional tomographic image data respectively with combining hydrogen oxidation calcium solid density ρ cHwith calcium carbonate solid density ρ caCO3, the gray-scale value of calcium hydroxide and calcium carbonate is calculated respectively with following formula:
Step 8: utilize following formulae discovery to obtain the three-dimensional spatial distribution of calcium carbonate volume content after different carbonization time:
f CaCO 3 1 ( x , y , z ) = C 1 reg ( x , y , z ) - G 0 ( x , y , z ) G CaCO 3 - ( 1 - 38 369 ) G CH
f CaCO 3 2 ( x , y , z ) = G 2 reg ( x , y , z ) - G 0 ( x , y , z ) G CaCO 3 - ( 1 - 38 369 ) G CH .
2. the quantitatively characterizing method of calcium carbonate space distribution in carbonization cement-based material as claimed in claim 1, it is characterized in that, cement-based material described in step 1 comprises clean slurry, mortar or concrete.
3. the quantitatively characterizing method of calcium carbonate space distribution in carbonization cement-based material as claimed in claim 1, it is characterized in that, Carbonization Conditions described in step 3 is carbon dioxide concentration expressed in percentage by volume is 10%-100%, and relative humidity is 60%-80%, and temperature is 20-60 DEG C.
4. the quantitatively characterizing method of calcium carbonate space distribution in carbonization cement-based material as claimed in claim 1, it is characterized in that, x-ray tomography wherein adopts medical, industrial, micro-or nanometer x-ray tomography equipment.
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CN106706679A (en) * 2016-11-30 2017-05-24 东南大学 Nondestructive test method for representing sizes of all carbonized zones of cement-based material
CN107271460B (en) * 2017-04-20 2020-07-31 东南大学 Quantitative characterization method for spatial distribution of internal moisture saturation change of porous material
CN110907631A (en) * 2019-12-13 2020-03-24 哈尔滨工业大学 Device for monitoring cement-based material carbonization degree and volume deformation and measuring method thereof
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