J. Ind. Eng. Chem., Vol. 13, No.

7, (2007) 1103-1108

Analysis of Microstructure and Properties of Autoclaved Aerated Concrete Wall Construction Materials
Yothin Ungkoon, Chadchart Sittipunt*, Pichai Namprakai, Wanvisa Jetipattaranat**, Kyo-Seon Kim***, and Tawatchai Charinpanitkul****,
Division of Energy Technology, School of Energy Environment and Materials, King Mongkuts University of Technology Thonburi, Bangmod, Rasburana, 126 Pracha U-thit Rd., Thungkru, Bangkok 10140, Thailand *Department of Civil Engineering, Faculty of Engineering, Chulalongkorn University, Phayathai Rd., Phathumwan, Bangkok 10330, Thailand **Research Development Center, Superblock Public Co., LTD, 9/1 Moo 11, Singburi Pak Dong Rd., Bangrachan, Kai Bangrachan, Singburi 16150, Thailand ***Department of Chemical Engineering, Faculty of Engineering, Kangwon National University, Chuncheon 200-701, Korea ****Center of Excellence in Particle Technology, Faculty of Engineering, Chulalongkorn University, Phayathai Rd., Phathumwan, Bangkok 10330, Thailand Received July 11, 2007; Accepted November 9, 2007

Abstract: Microstructure analyses in non-autoclaved aerated concrete (Non-AAC) and autoclaved aerated concrete (AAC) were conducted using optical microscopic and scanning electron microscopic (SEM) methods, while their chemical analyses were also carried out using X-ray diffraction (XRD). Laboratory investigation including physiothermal properties and field tests using four lab-scale houses built with the Non-AAC and AAC blocks were also compared. It could be observed that the AAC exhibited properties superior to that of the Non-AAC. Interestingly, the AAC blocks could provide lower humidity accumulation than the Non-AAC blocks, resulting in possibility to prevent mold growth in such construction materials. Keywords: autoclaved aerated concrete, microstructure, tobermorite

Introduction
1)

At present, construction works, such as high-rise buildings or offices and residential houses, in many countries including Thailand are growing very fast every year. Concrete has mainly been used as fundamental construction material for most of residential building because of its outstanding mechanical properties, low cost and availability. However, structure and foundation of buildings tend to become larger due to an increase in their scale, leading to much more time-consumption and cost. In monsoon region including the Southeastern Asian countries, the ambient condition is hot and humid so that

To whom all correspondence should be addressed. (e-mail: ctawat@chula.ac.th)

accumulation of heat and moisture in building wall plays an important role in its maintenance and energy conservation. As a result, ventilating fans and air-conditioners have been employed to remove heat for providing comfortable environment for residents. Meanwhile, both the economic and energy crisis has stimulated awareness of energy conservation, resulting in a drastic increase in studies on construction material which incorporates energy conservation. It should be noted that an approach which has been used in Civil Engineering works is the usage of construction materials as an insulator to prevent heat transfer from outsides of buildings. Khedari and coworkers reported that internal structure of concrete consisting of coconut and durian fibers mixed with cement and sand at various proportions could exhibit light weight characteristics [1,2]. They revealed that low density and thermal conductivity of blocks consisting of ad-

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Yothin Ungkoon, Chadchart Sittipunt, Pichai Namprakai, Wanvisa Jetipattaranat, Kyo-Seon Kim, and Tawatchai Charinpanitkul

ditive fibers could help prevent heat transfer into building. However, because of their low compressive strength, they could only be recommended to use for non-load bearing concrete masonry units. John and coworkers conducted an assessment of degradation on a wall panel composite made of low alkaline, clinker free, activated slag cement reinforced with coconut fibers [3]. Though the low alkaline cement was not able to prevent decomposition and leaching of lignin contained in the fibers, the leaching of lignin exerted insignificant effect on the wall performances. Meanwhile, various studies on non-autoclaved and autoclaved light weight concrete which consisted of cement and some other additives, such as ash, zeolite or polystyrene foam were also conducted to elucidate their structures and engineering properties [4-6]. For instance, effect of polymer cement modifiers on mechanical and physical properties of mortar using waste concrete fine aggregate was investigated and found that porosity of the mortar could be increased by addition of higher contents of polyacrylic ester (PAE) modifier [7]. Such polymeric modifier could lead to enhanced performance in hot water resistance and higher compressive strength but worse flexural strength [8]. There are two types of autoclaved aerated concrete (AAC) production methods which are chemical and mechanical processes. In the chemical process, some metallic compounds would be added to react and generate tremendous amount of air bubbles in concrete texture while in mechanical process expansive foaming agent is normally employed. In general, AAC could be prepared in a high pressure autoclave under conditions of temperature o and pressure higher than 180 C and 12 bar, respectively [5]. Approximately the porosity is 80 % of the volume of the processed cement, resulting in its very light weight. Additionally, AAC has excellent properties of acoustic insulation, fire resistance and allergy-free while it tends to suffer edge damage or breakage if it is subject to abrasion or collision. In order to produce more promising AAC, various researches on its physical structure have been initiated using microscopic analyses and X-ray diffraction (XRD) to investigate their chemical and structural characteristics [9-13]. To our knowledge, there are very few systematic investigations on thermal and physical properties of AAC in Thailand. So far, only some comparisons of engineering and thermal properties of clay bricks, concrete blocks, AAC and Non-AAC have been reported [14,15]. Studies on thermal inertia of concrete blocks by Ropelewski and coworkers [16] and Ungkoon and coworkers [17] are involving with heat transfer by radiation to buildings made of AAC and Non-AAC. It was found that Non-AAC blocks with higher density are likely to be able to transfer heat faster than the lighter AAC and in turn lead to shorter delay time in heat transmission. Ungkoon and cow-

orkers has also conducted a study on moisture and thermal resistance of building walls made of AAC blocks and clay bricks [18]. Their experimental results showed that the wall made of AAC could resist moisture and reduce heat transfer due to its inner porous structure. However, there is insufficient understanding of microstructure which could affect on thermal properties of AAC. Therefore, this work sets its aim at examining the porous structure of both AAC and Non-AAC in order to elucidate the formation process of their microstructures using optical microscopy and scanning electron microscopy (SEM). Also chemical and structural analyses are conducted using X-ray diffraction (XRD) to Figure out the effect of their composition on their thermal properties. Comparison of thermal and mechanical properties of AAC and Non-AAC has also been reported.

Materials and Method

Specimens of AAC were collected from a manufacturer which has been certified by Thailand Industrial Standard (TIS) 1505-2541. 120 pieces of AAC blocks with a uniform size of 200 600 75 mm were randomly sampled for investigation. Meanwhile, the Non-AAC blocked of the same size and amount manufactured at the same factory were sampled for comparison. Both AAC and NonAAC specimens were subjected to tests as follows; 1) Thailand Industrial Standard (TIS) 1505-2541 and Din 4165-1986 for determining dry density, compressive strength, and flexural strength, 2) JIS A 2618 standard for examining thermal conductivity using Thermal Conductivity Tester (model 88 K-FOTOR, ANACON), 3) DSC analysis for determining specific heat capacity using a differential scanning calorimeter (Model DSC 7), 4) microscopic analysis using scanning electron microscopy (SEM, Model JEOL JSM 5800 equipped with Energy Dispersive Spectroscope), and 5) chemical analysis using XRD (X-ray Diffractometer, model Bruker D8).

Results and Discussion

In general, it is known that tobermorite with orthorhombic structure could be stable with Ca/Si ratio of 0.8 1.0 and temperature of ambient condition up to 150 o C. It generally coexists within tetrahedral silicate layers and octahedral calcium layers [17]. With hydrothermal reaction between SiO2 and Ca(OH)2 a system of Calcium-Silicate-Hydrate (so-called C-S-H system) could be formed as slurry phase by following a two-step process. In the first step, calcium silicate hydrate gel (C-S-H gel) will be generated on the surface of SiO2 and then react with Ca(OH)2 to form well-organized crystal-

Analysis of Microstructure and Properties of Autoclaved Aerated Concrete Wall Construction Materials

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Figure 1. Model of Tobermorite structure consisting of protonated silicate ions and water.

line [19]. In the second step, curing of crystalline product would be taken into account. There are two alternatives of curing process which could provide specimen of different properties. The first curing process making use of air to cure specimens could create hydrogarnet crystalline of which the structure would strongly depend on curing time period. The other is an autoclave curing process in which high pressure and temperature would be applied to the specimens. At a pressure of 1012 bars and a temperature of 180190 oC, tobermorite could be formed in the specimens. As depicted in Figure 1, the tobermorite structure model consists of Ca2+ ions which are entrapped in the protonated silicate ions [9]. Therefore, the tobermorite crystal is stable to carbonation reaction under the condition of ambient temperature and the pressure but it will be disintegrated at the temperature higher than 650 oC. From the SEM investigation on the surface morphology of the two typical samples of light weight AAC and Non-

AAC blocks, it could clearly be observed that the surface of Non-ACC sample consisted of large pores while the ACC sample exhibited smoother surface with much smaller porosity as shown in Figure 2. For further investigation on the porous structure of typical samples of Non-AAC and AAC, SEM micrographs with higher magnification shown in Figure 3 are taken into account. In Figure 3(a) Non-AAC samples consist of particulate clusters of evenly distributed sizes, which situate around craters generated by the existence of uncontrollable air bubbles in curing process. It could further be observed that the crystallinity of the Non-AAC was resulted from random formation of gas bubbles, leading to formation of cavities with various depths. Also seen in Figure 3(a), some cracks observed on the Non-AAC surface would possibly lead to a decrease in the mechanical strength because they could become sources of fatigue growth. On the other hand, Figure 3(b) revealed the samples of AAC exhibit smoother surface with some porosity and particulate of narrower size. It is notable that there are no cracks observed on the surface of denser AAC samples. This could be implied that under high pressure and temperature in autoclaving process, denser phase of C-S-H could be formed. For further investigation of their crystallinity, SEM micrographs with further higher magnification were employed. Figure 4(a) clearly reveals that Non-AAC samples are comprised of particulate calcium silicate of unevenly distributed morphologies. Primary particles existing in the Non-AAC samples exhibit average size of 200 400 nm. Sub-micron particulates gathering as agglomerates with average size of 5 m could form loose matrix surrounding by voidage, resulting in lower density and thermal conductivity of the Non-AAC samples. However, considering Figure 4(b), one could clearly observe

(a)

(b)

Figure 2. SEM micrographs of non-AAC and AAC specimens.

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Yothin Ungkoon, Chadchart Sittipunt, Pichai Namprakai, Wanvisa Jetipattaranat, Kyo-Seon Kim, and Tawatchai Charinpanitkul

(a)

(b)

Figure 3. Comparison of surface morphology of Non-AAC and AAC specimens.

(a)

(b)

Figure 4. Comparison of crystalline structure of Non-AAC and AAC specimens.

Figure 5. XRD patterns of (a) Non-AAC and (b) AAC specimens (Q: quartz , T: tobermorite and C: calcite).

that finer needle-like crystalline structures exist thoroughly the surface of AAC samples. The average size of

sub-micron needle crystal is ca. 400 nm with aspect ratio of 2030. Tremendous amount of finer porosity within the matrix of fine particulate would also result in much lower specific density of AAC samples. In order to confirm the crystal structure of both Non-AAC and AAC samples, XRD analysis was also carried out. XRD patterns in Figure 5 reveals that Non-AAC samples mainly consist of calcite and quartz. Meanwhile, in AAC sample main product is crystalline in as much as tobermorite and quartz are present. With a high pressure of 12 bar and o temperature of 180200 C, calcite in the tested specimens could undergo phase transformation process to become tobermorite. Such experimental results are in a good agreement with those previous reports [9-11]. Difference in such crystal morphologies and phases in Non-AAC and AAC samples are supposed to exert significant effects on not only mechanical but also thermal characteristics of the samples. Accordingly, 250 pieces of Non-AAC and AAC samples were randomly collected

Analysis of Microstructure and Properties of Autoclaved Aerated Concrete Wall Construction Materials Table 1. Mechanical and Thermal Characteristic Test of Non-AAC and AAC Samples
Characteristics of sample tested Density (kg/m ) Compressive strength (MPa.) Flexural Strength (MPa.) Thermal conductivity (W/mC) Heat capacity (J/kgK.)
3

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Min 733 1.6 0.55 0.179 1,303

NonAAC Max 750 1.7 0.64 0.189 1,595

Avg. 741 1.6 0.59 0.184 1,449

Min 573 3.7 0.90 0.132 1,193

AAC Max 577 4.8 1.23 0.135 1,256

Avg. 575 4.3 1.06 0.133 1,224

for the statistical test of their mechanical and thermal characteristics. Table 1 summarizes the mechanical and thermal investigating results. It could be clearly observed that AAC samples exhibit specific density almost 20 percent lower than that of Non-AAC. Meanwhile, average compressive and flexural strength of AAC samples are 2.7 and 1.8 times of those of Non-AAC, respectively. These superior mechanical properties of AAC could be attributed to the present of higher crystallinity of tobermorite phases in AAC samples [13,15]. On the other hand, it could also be seen that average thermal conductivity and heat capacity of AAC samples are significantly lower than those of Non-AAC. As could be confirmed by microscopic analyses, the existence of micro-sized porosity in AAC samples would lead to higher insulating performance. Moreover, it has been reported that AAC could also exhibit lower drying shrinkage when compared with Non-AAC [9]. Finally, field tests using four lab-scale houses built with the Non-AAC and AAC blocks were also carried out. Details of field test facilities are available elsewhere [18]. It could be observed that walls built with the AAC blocks could exhibit insulating and humidity adsorbing performance superior to that of a wall built with the Non-AAC blocks. Temperature in the houses built with the AAC blocks is significantly lower than that in the Non-AAC houses. Additionally, the AAC blocks could also provide lower humidity accumulation than the Non- AAC blocks, resulting in possibility to prevent mold growth in such construction materials. In summary, it could be confirmed experimentally that suitable treatment of aerated concrete specimens using autoclaving method could enhance phase transformation of calcite to tobermorite and control formation of microporosity in the cement matrix. The existence of crystalline tobermorite phase and microporosity, which are justified by microscopic and spectroscopic analyses, could enhance both mechanical and thermal properties of AAC specimens compared with those of Non-AAC. Based on these investigating results it is reasonable to recommend that AAC could be more suitable to apply as wall construction material which exerts superior mechanical strength with better insulating performance.

Conclusion
Under a condition of high pressure and temperature treatment, calcite in aerated cement specimens could undergo phase transformation process to become tobermorite, which is more stable than former phase. High pressure autoclaving could also control formation of evenly distributed micropores within the cement matrix. The existence of tobermorite phase in AAC plays an important role in providing various outstanding properties. With autoclaved aerating process, AAC sample exhibits lower density than that of Non-AAC. Additionally, AAC could exhibit superior compressive strength and thermal insulating properties. With a series of experiments it could be confirmed AAC could be employed as a promising concrete building material.

Acknowledgments
The authors gratefully acknowledge the Superblock (public) Co., Ltd. for financial support to this research work. T. C. would gratefully acknowledge financial support from Silver Jubilee Fund of Chulalongkorn University for CEPT. Support from the Ministry of Education and Human Resources Development (MOE) and the Ministry of Commerce, Industry and Energy (MOCIE) through the fostering project of the IndustrialAcademic Cooperation Centered University is also acknowledged.

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