X. HE et al.: EFFECT OF DRY-WET CIRCULATION ON THE MECHANICAL PROPERTIES AND PORE STRUCTURE ... 177–182 EFFECT OF DRY-WET CIRCULATION ON THE MECHANICAL PROPERTIES AND PORE STRUCTURE OF AUTOCLAVED AERATED CONCRETE VPLIV SUHO-MOKRE CIRKULACIJE NA MEHANSKE LASTNOSTI IN STRUKTURO POR V AVTOKLAVU PREZRA^ENEGA BETONA Xiao He, Jian Yin * , Jiewen Yang, Qiao Liang, Songyun Wu School of Civil Engineering, Central South University of Forestry and Technology, no. 498 Shaoshan South Road, Tianxin District, Changsha 410004, Hunan, China Prejem rokopisa – received: 2018-08-30; sprejem za objavo – accepted for publication: 2018-10-18 doi:10.17222/mit.2018.190 Dry-wet circulation is the main service environment for autoclaved aerated concrete. In this study, we looked at selected auto- claved aerated concrete with dry-wet circulation times of (0, 30, 60, 150, 270 and 340) min. The tested mechanical properties include the compressive strength and the splitting tensile strength. Scanning electron microscopy (SEM) and Image-Pro-Plus (IPP) software were chosen to quantitatively characterize the microstructure. The results showed that as the dry-wet circulation times increased, the compressive strength decreased after first increasing, and the splitting tensile strength reduced. In addition to the pore structure, microcracks and internal acicular ettringite were produced. The pore size distribution was concentrated from 1.0 mm to 1.5 mm, when dry-wet cycle times were 60 min or more. Keywords: autoclaved aerated concrete, dry-wet circulation, mechanical properties, Image-Pro-Plus, pore structure Suho-mokra cirkulacija je glavni naravni postopek za prezra~evanje betona v avtoklavu. Avtorji opisujejo prezra~evanje betona v avtoklavu s suho-mokro 0, 30, 60, 150, 270 in 340-minutno cirkulacijo. Vzorcem betona so nato dolo~ili mehanske lastnosti in sicer tla~no ter cepilno trdnost. Kvantitativno so okarakterizirali mikrostrukturo z vrsti~nim elektronskim mikroskopom (SEM) in programsko opremo za obdelavo slike Image-Pro-Plus (IPP). Rezultati ka`ejo, da z nara{~ajo~im ~asom suho-mokre cirkulacije tla~na trdnost po prvem dvigu v primerjavi z necirkuliranim betonom pade, cepila trdnost pa se zmanj{uje. V porozni strukturi betona so nastale mikrorazpoke in interni igli~asti etringit (hidroksidni Ca-Al sulfatni mineral). Porazdelitev velikosti por je bila koncentrirana med 1,0 in 1,5 mm po 60-minutnem ali {e dalj{em suho-mokrem ciklu. Klju~ne besede: v avtoklavu prezra~en beton, suho-mokra cirkulacija, mehanske lastnosti, obdelava slike s programsko opremo Image-Pro-Plus, struktura por 1 INTRODUCTION Autoclaved aerated concrete has good performance with respect to heat preservation and heat insulation, and also saves clay resources. The excellent properties of autoclaved aerated concrete depend on its unique pore structure. 1–4 But in the actual service process, dry-wet circulation causes deformation. Studies have shown that one of the main factors was the dry-wet circulation. 5–7 In addition, as the dry-wet circulation times increased, the performance of the heat preservation and heat insulation declined. Autoclaved aerated concrete, as a wall material, is often in the environment of rainfall infiltration and drying evaporation. Studies showed that dry-wet circu- lation speeded up the invasion rate of harmful media, such as sulfate and chloride, which lead to destruction, and also changed the moisture content for deformation. Autoclaved aerated concrete with the characteristics of dry shrinkage and wet expansion, for inflation happen when the internal moisture content increased, on the other hand, contraction was produced. Studies also showed that the humidity inside the autoclaved aerated concrete emerged to a graded distribution, and larger internal stress occurred and when the stress exceeds a certain limit, cracking of the autoclaved aerated concrete happened, which results in its unique pore structure being damaged, the mechanical properties declining, and life of service being reduced. 8–10 This paper studies the relationship between the me- chanical properties and the pore structure of the auto- claved aerated concrete under dry-wet circulation. Scanning electron microscopy (SEM) was used to characterize the micro-pore structure. By employing Image-Pro-Plus software to a binary image of the pore structure, we obtained a quantitative characterization of the pore structure, in order to calculate the pore diameter distribution. A fractal dimension was used to character- ize the pore size distribution, and the fractal dimension had a quadratic correlation with the mechanical proper- ties though the regression equation. Materiali in tehnologije / Materials and technology 53 (2019) 2, 177–182 177 UDK 620.1:67.017:691.32:542.468 ISSN 1580-2949 Original scientific article/Izvirni znanstveni ~lanek MTAEC9, 53(2)177(2019) *Corresponding author e-mail: csuyj700930@163.com 2 EXPERIMENTAL PART 2.1 Materials Autoclaved aerated concrete was obtained from Changle building materials co. LTD in Changsha, China. Table 1 shows the properties of the autoclaved aerated concrete. Table 1: Main properties of autoclaved aerated concrete Model Bulk density Intensity of average Size A3.5 B06 <625 >3.5 MPa (600 × 200 × 100) mm 2.2 Dry-wet circulation test methodologies The methods of the specimens’ processing and performance testing were referred to GB/T 11969-2008 "test methods of performance for autoclaved aerated con- crete". The dry-wet circulation of a specimen prepared with a sawing machine, chose a group based on the parts from the above, middle and below, for along the direc- tion of the gas, specifically included the above distance 30 mm from the top of the specimens, the block at the center of the products, and the block a distance 30 mm from the bottom. The size of the specimen was (100 × 100 × 100) mm and a group of specimens was three pieces. The chosen specimen was dried with an electric drum dryer to remain constant quality, then cooling to a temperature of 20±5 °C and maintained for 20 min. Next it was soaked in a water tank at a temperature of 20±5 °C, and the level of water exceeded the height of specimen by 30 mm, held for 5 min, then removed, and kept for 30 min at a temperature of 20±5 °C. Finally, in the selected electric drum dryer, it was dried for7hata temperature of 60±5 °C, then cooled for 20 min, later soaked in the water at a temperature of 20±5 °C, for one cycle. The selected times of the dry-wet circulation were (0, 30, 60, 150, 270 and 340) min. 2.3 Mechanical test methodologies The moisture in the specimen was maintained at 8 % to 12 %. The specific methods were as follows: chose the brush, evenly apply water on the specimen, then select the PP bag packaging specimen for1dat20°C,usethe water to achieved a uniform distribution, chose the uni- versal mechanical testing machine for testing the com- pressive strength and the splitting tensile strength. And the size of specimen was (100 × 100 × 100) mm 3 . 2.4 Pore structure test methodologies Scanning electron microscopy was chosen to observe the micropore structure of the autoclaved aerated con- crete, the size of test block was (10 × 10 × 10) mm 3 . Image-Pro-Plus software was selected for a binary image of the pore structure, so as to provide a calculated and quantitative characterization of the pore diameter distri- bution. 3 RESULTS AND DISCUSSION 3.1 Mechanical properties of autoclaved aerated con- crete under dry-wet circulation Figure 1 shows the compressive strength and splitt- ing tensile strength of the autoclaved aerated concrete under dry-wet circulation. When the dry-wet circulation increased, the tendency of the compressive strength and splitting tensile strength of autoclaved aerated concrete was to decrease after first increasing. With dry-wet cir- culation times of 30 min, the compressive strength was greater than the specimen with no dry-wet circulation. The compressive strength was 4.27 MPa, increased by 0.47 % compared to the no dry-wet circulation. As we continued to increase the times of dry-wet cycle, compressive strength showed a tendency to decline, such as with times of the dry-wet cycle equal to (60, 150, 270 and 340) min, its compressive strength was (4.24, 4.23, 4.16 and 3.99) MPa. When the dry-wet circulation times reached 340 min, the value of the compressive strength was the lowest, and had declined by 6.1 % compared to the no dry-wet specimen. The splitting tensile strength showed the same ten- dency as the compressive strength. When the dry-wet circulation times went up to 30 min, the splitting tensile strength reached a maximum of 0.568 MPa, compared to the no dry-wet circulation, it increased by 0.53 %. And with the dry-wet circulation times increased to (60, 150, 270 and 340) min, the value declined, respectively, to (0.563, 0.562, 0.556, 0.541) MPa. Compared with the specimen that had no dry-wet cycles, the splitting tensile strength declined by 4.24 %, when the dry-wet circul- ation times went to 340 min. The reason for this behavior was that with an increase in the times of dry-wet circulation, the moisture was made to move in and out of the specimen more X. HE et al.: EFFECT OF DRY-WET CIRCULATION ON THE MECHANICAL PROPERTIES AND PORE STRUCTURE ... 178 Materiali in tehnologije / Materials and technology 53 (2019) 2, 177–182 Figure 1: Effect of mechanical properties of autoclaved aerated con- crete under dry-wet circulation frequently. For the times of dry-wet circulation equal to 30 min, the influence of the hydration products on the sand particles was negligible, and hence the mechanical properties increased. As the dry-wet circulation times increased, the hydration products reacted further with the porous structure, thus resulting in a decrease in perform- ance. 3.2 Microstructure of autoclaved aerated concrete un- der dry-wet circulation Figure 2 shows SEM images of the autoclaved aerated concrete under dry-wet cycle times of 340 min, and respectively magnified by 1000 and 1600 times. According to Figure 2a the internal cracks of the specimen appeared, with those microcracks expanded into large cracks due to the external conditions, which resulted in a degradation of the macroscopic perform- ance, e.g., the strength and dynamic modulus of elasticity. Also, the generation of cracks erosion of other ions, caused further damage during the dry-wet circul- ation of the specimen. Figure 2b shows acicular ettringite, with the increased dry-wet circulation times, and the ettringite began to grow inside the crack, which results in the ettringite appearing in the pore structure. 3.3 Pore structure of autoclaved aerated concrete un- der dry-wet circulations 3.3.1 Characterizing methods for the pore structure By employing the technology of image analysis we analyzed the pore structure. Figure 3 shows the methods. First, smear the surface of autoclaved aerated concrete to the color of black, next binarization of the image through the soft of the Image-Pro-Plus, for the pore structure more clearly, then identify the pore structure with the X. HE et al.: EFFECT OF DRY-WET CIRCULATION ON THE MECHANICAL PROPERTIES AND PORE STRUCTURE ... Materiali in tehnologije / Materials and technology 53 (2019) 2, 177–182 179 Figure 3: Schematic diagram of autoclaved aerated concrete pore structure analysis Figure 2: Scanning electron microscopy images of the autoclaved aerated concrete under dry-wet circulation: a) magnified 1600 times, b) magnified 1000 times Image-Pro-Plus and count it. Finally, obtain the para- meter of the pore structure for the pore size. 3.3.2 Pore size distribution Figure 4 shows the distribution of the pore size. When the time of the dry-wet circulation was 0, the distribution of the pore size concentrate was 0.1–0.5 mm, and the ratio reached 48.25 %. With an increase of the dry-wet circulation times to 30 min, the pore size distribution was concentrate to 0.5–1.0 mm, the propor- tion was 46.09 %, and with dry-wet cycles times in- creased to (60, 150, 270 and 340) min, the aperture size concentrate was 1.0–1.5 mm, the percentage achieved was 35.14 %, 33.12 %, 34.23 % and 31.02 %, respect- ively. For the specimen that had no dry-wet circulation, the amount of pore size distribution that more than 1.5 mm is zero, and under dry-wet circulation, an aperture size distribution of 1.5 mm appeared, and the dry-wet circulation times reached to (60, 150, 270 and 340) min, X. HE et al.: EFFECT OF DRY-WET CIRCULATION ON THE MECHANICAL PROPERTIES AND PORE STRUCTURE ... 180 Materiali in tehnologije / Materials and technology 53 (2019) 2, 177–182 Figure 5: Fractal dimension of size pore distribution, a) to f) for dry-wet circulation of (0, 30, 60, 150, 270 and 340) min Figure 4: Pore size distribution of autoclaved aerated concrete under dry-wet circulation, a) to e) for dry-wet circulation times of (0, 30, 60, 150, 270 and 340) min and the proportion, respectively, of 29.24 %, 39.70 %, 42.38 % and 39.70 %. 3.3.3 Fractal dimension of the pore size distribution We used the method of box-counting dimension. The specific method was as follows: chose a square with side length of r to cover the pore, and statistically the number of the square is N (r), by changing the side length of the square, the statistical number corresponds to the square, obtained a series of corresponding points, the slope is the fractal dimension for D c . Equation (1) was used for the fractal dimension. D Nr r c d d = (ln ( )) (ln ) (1) The fractal dimension of the pore size distribution characterization for the uniformity of the pore size was shown in Figure 5, when dry-wet circulation times of (0, 30, 60, 150, 270 and 340) min, the fractal dimension of the pore size distribution was 1.41, 1.45, 1.51, 1.52, 1.56 and 1.64. Figure 6 shows the relations between the fractal dimension of the pore size distribution and the mecha- nical properties. The research showed the relations among the fractal dimension of the pore size distribution with the compressive strength and the splitting tensile strength. The results present a good quadratic correlation of the fractal dimension and the mechanical properties though the regression equation. The value of the fractal dimension increased, the compressive strength and splitting tensile strength tended to decrease. The result implies that the pore size distribution has an influence on the mechanical properties. 4 CONCLUSIONS Dry-wet circulation is one of the most severe environmental conditions. The relationship between the mechanical properties and the pore structure of auto- claved aerated concrete under dry-wet circulation is discussed in this study. When the times of the dry-wet circulation increased, the compressive strength decreased after first increasing and the splitting tensile strength declined. For dry-wet circulation times of 340 min, the compressive strength and the splitting tensile strength were 3.99 MPa and 0.541 MPa, and reduced by 6.1 % and 4.24 %, compared to the no dry-wet circulation. The microstructure of the autoclaved aerated concrete under dry-wet circulation was obtained by SEM, and the results showed that ettringite emerged. Less ettringite may lead to better mechanical properties, but more can break the pore structure, and reduce the properties. For a quantitative characterization of the pore structure we used a binary image and Image-Pro-Plus for a clear pore structure. Then we calculated the pore diameter distribu- tion, and compared the pore structure of the autoclaved aerated concrete under a dry-wet cycle. We chose the fractal dimension to characterize the pore size distribu- tion and the value of the fractal dimension increase with the time of dry-wet circulation increase. The pore size distribution was found to affect the mechanical proper- ties. Acknowledgments This research was supported by National Key R&D Program of China (no. 2016YFC0700801-01). 5 REFERENCES 1 K. G. Wakili, E. Hugi, E. Karvonen, L. Karvonen, P. Schnewlin, F. 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