Cerâmica 67 (2021) 370-377 ...

370 Cerâmica 67 (2021) 370-377 http://dx.doi.org/10.1590/0366-69132021673833118

INTRODUCTION

Portland cement concrete is the most important building material of modern civil construction and the second material largest used on Earth, only after water [1-4]. Some problems during the mix design and execution of concrete mixtures can cause concrete damage and diminish concrete durability. The cracks in concrete are generated due to different environmental exposition, for example, by shrinkage, extreme mechanical loading, aggressive environment contact, or environmental weathering [5-7]. Cracks are undesirable because they reduce the toughness of concrete and are pathways to aggressive agent entrance, such as water, oxygen, and CO2, which can damage the reinforcing steel, decreasing the structure lifespan [7-9]. Furthermore, crack repair works are expensive and increase the carbon footprint [10].

Self-healing concrete (SHC), also known as self-repairing concrete, is an alternative to improve the durability of concrete structures because it is a material able to automatically seal their eventual cracks without the need for external work [4, 11]. The use of SHC can save costs associated with repair works and improve the safety, lifespan, and sustainability of concrete structures [5, 12-14]. There are two types of self-healing mechanisms: autogenous and autonomous. Studied since the nineteenth century, autogenous self-healing designates the ability of concrete to self-heal fine small cracks with compounds present in its composition reacting

with water, without external operations. Autonomous self-healing is associated with the presence of unusual materials in the cement matrix, such as by encapsulation of healing agents or capsules containing bacteria [15-20]. The type of materials and their proportions influence the effectiveness of autogenous healing [2]. Takagi et al. [21] made SHC using a 392 kg/m3 of cement content, with crystalline admixture (2.5% by weight of cement) and fiberglass. They reported that the type of cement, blast furnace slag, and crystalline admixture contents influenced the self-healing effect. Reddy and Ravitheja [19] used a cement content of 425.5 kg/m3 in SHC with crystalline admixture. They stated that the SHC recovered the compressive and tensile strengths even cured in different conditions (water immersion, wet-dry cycles, water contact, and air exposure). Roig-Flores et al. [22] proposed two types of SHC with cement contents of 275 and 350 kg/m3 and used 4% crystalline admixture by weight of cement; test results showed that both concretes presented a similar healing behavior, with a positive effect of water immersion curing at 30 °C. Azarsa et al. [12] used a cement content of 358 kg/m3 with a crystalline admixture content of 2% by weight of cement and found that the admixture was efficient in decreasing the permeability.

Based on these researches, it was observed that cement content can affect concrete durability [23]. In this way, the objective of this article was to study the influence of cement content on some properties of an autogenous SHC. SHC was prepared with a commercial crystalline admixture, a permeability-reducing agent composed of reactive silica and crystalline catalysts, which chemically reacts with Ca(OH)2 in the presence of water, providing crystal growth and crack filling [12, 13, 24, 25].

*[email protected]://orcid.org/0000-0003-0536-7621

Self-healing concrete with crystalline admixture made with different cement contentR. H. Geraldo1,2*, A. M. Guadagnini1, G. Camarini2,3

1Facens University, Rod. Sen. José Ermírio de Moraes 1425, 18087-125, Sorocaba, SP, Brazil2University of Campinas, School of Civil Engineering, Architecture and Urban Design, 13083-889,

Campinas, SP, Brazil3University Center of Minas South, 37031-099, Varginha, MG, Brazil

Abstract

Self-healing concrete (SHC) is obtained with self-healing agents, which can seal small cracks without additional repair works, improving concrete durability. The present paper studied the influence of cement content (450, 475, and 500 kg/m3) on mechanical properties (compressive and tensile strength) and porosity (capillary water absorption, water absorption, and void index) of SHC with crystalline admixture. A crack induction was carried out in SHC, and the results were compared with two reference concretes (with and without crack induction). SHC had similar compressive strength with reference concrete made without crack induction, independently of cement content. Water absorption and void index of SHC decreased with higher cement content, and a significant reduction of capillary water absorption was found after 90 days. The crystalline admixture was very efficient in decreasing concrete porosity mainly at longer ages. SHC made with high cement content developed a higher porosity reduction.Keywords: self-healing concrete, crystalline admixture, autogenous healing, durability.

371 R. H. Geraldo et al. / Cerâmica 67 (2021) 370-377

EXPERIMENTAL PROCEDURE

Materials: high initial strength Portland cement (CPV-ARI) was used, which is equivalent to ASTM type III. CPV-ARI was employed because it has a high clinker content and high heat release [26]. So, this type of cement can be liable to crack by thermal shrinkage. Locally available river quartz sand and basaltic crushed stone were used as fine and coarse aggregates, respectively. Fig. 1 and Table I show, respectively, the particle size distribution curves (sieve analysis) of aggregates and their physical properties. Commercial crystalline admixture and alkali-resistant fiberglass with 12 mm length were employed to promote, respectively, the self-healing process and the control of crack size. The crystalline admixture content was 2% by weight of cement, recommended by the admixture producer. A polycarboxylate-based superplasticizer was used as a water reducer admixture. The water used was from the municipal supply with the following physical-chemical characteristics: 50 mg/L chloride, 0.75 mg/L

fluoride, 8.65 mg/L sodium, 3.6 mg/L sulfate, 0.36 NTU of turbidity, and pH 6.99. Table II presents the chemical compositions by X-ray fluorescence (XRF) spectroscopy (Supermini200, Rigaku) of Portland cement and crystalline admixture. The results showed that both materials were mainly composed of CaO and SiO2, oxides that corresponded to more than 70% of the total. The Na2O content in crystalline admixture was more than four times higher than that observed in Portland cement. The values of the specific mass of Portland cement and crystalline admixture were 3120 and 2900 kg/m3, respectively.

Experimental mixtures: all concretes were designed as self-compacted concretes. Before producing the concrete for the experimental research, an initial attempt was made with a cement content of 400 kg/m3, but the concrete did not have any flow. On the other hand, increasing the cement content to 500 kg/m3 segregation occurred during the slump flow test. To maintain similar water and superplasticizer contents, it was chosen to make the concretes with three cement contents: 450, 475, and 500 kg/m3 (Table III). The mortar content was the same in all the mixes. The high cement contents were chosen to deal with situations more vulnerable to generate cracks by heat releasing, once thermal and drying shrinkage are more pronounced as the cement content increases [31]. These three mixtures (Mix 1, Mix 2, and Mix 3) were used to make the concretes used in the experimental work.

Specimens preparation and curing: concrete mixtures were made following the same procedure. The materials (Table III) were mixed in a concrete-mixer (inclined shaft) until complete homogenization. Cylindrical specimens were cast (100 mm diameter and 200 mm height) and after 48 h in molds, the specimens were demolded and stored for 5 days in a wet chamber (22 °C and relative humidity of 95%). Some of the specimens had a crack induction process at 7 days, which is commonly used to test the healing efficiency [22, 25, 32, 33]. After the cracking process, all the specimens were immersed in water until testing age. The water immersion favors the self-healing process, accelerating the sealing of cracks [6, 14]. The concrete specimens were submitted to three Figure 1: Particle size distribution curves of the aggregates.

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Component CaO SiO2 Fe2O3 Al2O3 SO3 SrO Na2O Others LOI

PC 63.47 14.50 6.18 4.25 3.72 1.01 0.79 2.11 3.97CA 59.80 13.00 6.30 4.56 2.72 1.15 3.34 2.73 6.40

LOI: loss on ignition.

Table II - Chemical compositions (wt%) of Portland cement (PC) and crystalline admixture (CA).

Table I - Physical properties of the fine and coarse aggregates.

Property Coarse Fine StandardFineness modulus 6.74 1.59 NBR NM 248 [27]

Maximum diameter (mm) 12.50 0.60 NBR NM 248 [27]Specific gravity (kg/m3) 2640 2590 NBR NM 52/53 [28, 29]

Bulk density (kg/m3) 1367 1381 NBR NM 45 [30]

372R. H. Geraldo et al. / Cerâmica 67 (2021) 370-377

different conditions, as follows (Fig. 2): condition 1, REF - reference concrete; condition 2, REF-CI - reference concrete with crack induction: at the age of 7 days, the concrete was submitted to a compressive load of 90% of the ultimate strength at 7 days; the load was applied for 2 min with the purpose of generating micro-cracks in concrete (crack induction); and condition 3, SHC-CI - self-healing concrete with crystalline admixture and with crack induction (similar to REF-CI, Fig. 3). The crack induction was made with specimens at 7 days to obtain indications about the crystalline admixture performance in sealing possible cracks that originated at the early ages

of the concrete. The time of load application (2 min) was defined according to the study of Takagi [34].

Test methods: concretes were subjected to tests of: flow (just after mixing), compressive strength, tensile strength (Brazilian test), capillary water absorption, total water absorption, and void index. In the hardened state, the specimens were tested after cracking and curing (Fig. 4). Flow test: concrete fluidity was determined by the slump-flow test immediately after the concrete mixing. To this test, a rigid metallic plate was put in a flat place and the slump cone was fulfilled with concrete without any vibrating. Thereafter, the cone was vertically removed, and the concrete was spread on the plate. The test was made according to NBR 15823-2 standard [35] and it was considered the average value of the three diameters measured in the spread concrete. This test is common to self-compacting concretes and it was made due to the high fluidity of the concrete mixtures. Compressive and tensile strength tests: compressive strength and tensile strength (Brazilian test, Fig. 5) were made according to NBR 5739 [36] and NBR 7222 [37] standards, respectively. Three cylindrical specimens (100 mm diameter x 200 mm height) of each mixture and condition were evaluated at the ages of 28 and 90 days. After 25 and 87 days, the specimens were removed from the water, oven-dried for 72 h (105±2 °C), and allowed to cool at room temperature prior to the test. The mechanical tests were conducted on a Dinatest machine (F-250C-LCI, maximum load of 1112 kN).

Capillary water absorption test: capillary water absorption was measured in cylindrical specimens (100 mm diameter x 200 mm height). Three specimens of each condition and mixture were molded by each testing age (28 and 90 days). The test was made in accordance with NBR

Figure 3: Image of a concrete specimen after loading.

Table III - Concrete mix design (kg) for mixes with different cement content.

ComponentCement content (kg/m3)

Mix 1 Mix 2 Mix 3450 475 500

Portland cement 1 1 1Fine aggregate 1.87 1.68 1.51

Coarse aggregate 1.65 1.54 1.44Water 0.55 0.55 0.55

Crystalline admixture 0.02 0.02 0.02Superplasticizer 0.01 0.01 0.01

Fiberglass 0.002 0.002 0.002

Figure 2: Different mixes and conditions studied. Figure 4: Flowchart of test methods.

Figure 5: Scheme of tensile strength ‘Brazilian test’.


9779 standard [38] with some modifications, as follows. After 25 and 87 days, the specimens were removed from water and oven-dried (105±2 °C) for 72 h before testing. Afterward, the specimens had their lateral surface sealed so that the water flow was only uniaxial and perpendicular to the cross-sectional area. The sealed specimens were placed on thin supports in a tray such that their bottom surface was submerged, and it was in contact with water at a constant depth of 5±1 mm. The specimens were removed from the tray and weighed at different time intervals to evaluate the mass gain: 5, 10, 15, and 30 min and 1, 2, 4, 6, 8, and 24 h. Capillary water absorption at 28 and 90 days was calculated by:

Cwa = (Hm - Dm)/S (A)

where Cwa is the capillary water absorption (kg/m2), Hm is the humid mass (kg), Dm is the oven-dried mass (kg), and S is the cross-sectional area of the specimen (m2). Immediately after the capillary water absorption test, the specimens were broken, and the height of the water rise was measured with a digital caliper at both internal surfaces.

Total water absorption and void index tests: in this test, it was determined dry and saturated weights, as follows. The total water absorption and void index were determined at 28 and 90 days in cylindrical specimens in accordance with Brazilian standard NBR 9778 [39]. Before testing, the specimens were oven-dried for 72 h (105±2 °C) and weighed (dry weight - WDry). After drying, using a hydrostatic scale, the specimens were immersed in water for 72 h at room temperature (25±1 °C) and weighed (immersed weight - WIm). The saturated weight (WSat) was obtained by removing excess water from the specimen surfaces with a cloth and weighing. The results were obtained by:

Wa = [(WSat – WDry)/WDry].100 (B)

Vo = [(WSat – WDry)/(WSat – WIm)].100 (C)

where Wa is the water absorption (%), Vo is the void index (%), WSat is the specimen saturated mass after immersion (kg), WDry is the specimen oven-dried mass (kg), and WIm is the specimen immersed mass (kg).

RESULTS AND DISCUSSION

Slump flow: Fig. 6 shows the flow results of concretes obtained by the slump-flow test. The specimens had high fluidity that increased as the cement content increased. This occurred because a higher cement content improves the superplasticizer effect, dispersing the cement grains [40]. The concretes presented considerable values of spreading, acceptable for some types of self-compacting concretes [35]. Visual stability was observed in all the mixtures (no segregation). Crystalline admixture resulted in a low flow reduction when compared to the reference concrete (REF). Helene et al. [33] reported that concretes made with or

without the crystalline catalyst achieved similar slump values. Differently, Azarsa et al. [12] and Oliveira et al. [41] observed a decrease in a concrete slump value with the crystalline admixture addition. According to Azarsa et al. [12], the lower fluidity is related to the hydrophilic nature of crystalline admixture, which absorbs more water.

Compressive and tensile strengths: Fig. 7 shows the compressive and tensile strength results, which had no changes from 28 to 90 days, showing that the maximum strengths were already achieved at 28 days face to the use of high initial strength Portland cement. There were low differences among REF, REF-CI, and SHC-CI values. In both ages (28 and 90 days), the compressive strength of specimens with 500 kg/m3 cement content was higher than the other ones. The tensile strengths of specimens with 475 and 500 kg/m3 cement contents were similar. REF with 475 kg/m3 of cement had slightly higher results than other contents. The specimens achieved compressive and tensile strength values ranging from 50 to 65 MPa and 2.5 to 4.5 MPa, respectively. Reddy and Ravitheja [19] reported SHC with compressive and tensile strengths of around 44 and 3.3 MPa, respectively, at 28 days (SHC made with 425.5 kg/m3 cement content, crystalline admixture equal 1.1% of the cement weight, and cured in water immersion). In both studies, the results indicated that tensile strength was lower than 10% of compressive strength. The literature indicated a great potential of crystalline admixture to maintain or recover (when submitted to cracking induction) the compressive strength. Roig-Flores et al. [22] reported an increase of 15% in compressive strength with crystalline admixture addition; however, they used a higher content than this work (4% of the cement weight), and when it was considered the standard deviation, the compressive strengths of both concretes were very close. Pazderka and Hájková [42] also reported that concrete made with crystalline admixture addition (2% of the cement weight) had similar compressive strength with the reference concrete.

Capillary water absorption: Fig. 8 shows the capillary water absorption results of the concretes prepared with 400, 475, and 500 kg/m3 cement content at 28 and 90

Figure 6: Results of concretes’ flow.

450Cement content (kg/m3)

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m)

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00475 500


days. Capillary water absorption of SHC-CI at 90 days was the lowest one regardless of the cement content. The results showed a decrease in capillary suction on SHC-CI concrete from 28 to 90 days, which is an indication of healing efficiency [43]. The hydration products formed by the catalyst admixture results in microstructure densification and it decreases the capillary suction [5] (Fig. 9). SHC-CI concrete had a decrease in the pore interconnection with age. REF and REF-CI also had a decrease in capillary water absorption with age; however, it was lower than that registered by SHC-CI. The capillary water absorption of SHC-CI concrete after 24 h diminished with cement content from 28 to 90 days: 44% (450 kg/m3), 53% (475 kg/m3), and 33% (500 kg/m3). This may have occurred due to the continuity of healing effect over time, which was more pronounced at 90 days.

Fig. 10 shows the water penetration depth after the capillary water absorption test. Results showed REF had an increase in water penetration depth from 28 to 90 days, while REF-CI and SHC-CI presented a decrease with age. SHC-CI concrete at 90 days had a reduction of the water penetration depth in the range of 8% (450 kg/m3), 1% (475 kg/m3), and 8% (500 kg/m3) when compared to REF. Regardless of the cement content, the results of capillary water absorption and water penetration depth of concrete specimens from 28 to 90 days showed that: in REF concrete, the capillary suction increased; in REF-CI concrete, the capillary suction

decreased, even without using a self-healing agent, but it presented the highest water internal rise values; and SHS-CI concrete had the highest decrease in capillary suction and the lowest water penetration depth, regardless the cement content. The internal pore arrangements of concretes are influenced by the cracks, affecting the capillary water absorption [44]. The higher reduction of the water rise observed by SHC-CI even with crack induction is relevant and it indicated a disconnection of the capillary network [45].

Total water absorption and void index: Fig. 11 shows the results of total water absorption and void index of concrete specimens at 28 and 90 days. The results of total water absorption and void index indicated that the cement content influenced the porosity of the samples. According to Mehta and Monteiro [46], a higher cement content contributes to a lower porosity; however, the concrete of 475 kg/m3 cement content resulted in lower total water absorption and void index at 28 and 90 days than the concrete of 500 kg/m3. Considering the concrete of 450 kg/m3, the total water absorption and void index of REF were lower than REF-CI and SHC-CI, showing that with this cement content the crystalline admixture effect was not enough to decrease the concrete porosity. On the other hand, concretes of 475 and 500 kg/m3 cement content showed a strong effect of crystalline admixture at 90 days. SHC-CI concrete with 500 kg/m3 cement content presented

Figure 7: Results of compressive (a,b) and tensile (c,d) strengths of concretes at 28 and 90 days.

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a reduction in total water absorption of 47% and 58% when compared to REF and REF-CI, respectively. Azarsa et al. [12] reported a decrease of 50% in water penetration depth by using crystalline admixture. REF-CI concrete had the highest water absorption possible due to the crack induction applied in the specimens. The crack formation increases the permeability of concrete [17]. Comparing the results of REF-CI with SHC-CI, it was clear the favorable effect of crystalline admixture in decreasing the concrete porosity, mainly with a cement content of 500 kg/m3. As explained by Roig-Flores et al. [22] and Reddy and Ravitheja [19], a crystalline admixture has hydrophilic properties, increases the density of C-S-H, and decreases the concrete permeability. The low permeability improves the concrete durability [46]. The obtained results showed the efficiency of crystalline admixture as a self-healing agent mainly with the highest cement content analyzed (500 kg/m3).

Figure 8: Results of capillary water absorption of specimens made with cement contents of 450 kg/m3 (a,b), 475 kg/m3 (c,d), and 500 kg/m3 (e,f).

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Figure 9: Image of a concrete section showing cracks filled with hydration products.


Figure 10: Results of water penetration depth after the capillary water absorption test.

Figure 11: Results of total water absorption and void index at 28 and 90 days.

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Rajczakowska et al. [15] showed that the high availability of anhydrous cement, provided by high cement content, was not enough for autogenous self-healing. So, the results of porosity tests indicated crystalline admixture had an important role and the increase in cement content also contributed to the healing process.

CONCLUSIONS

The effect of cement content (450, 475, and 500 kg/m3) on the properties of self-healing concrete (SHC) was evaluated. From the obtained results, the following conclusions can be drawn. The increase of cement content resulted in a higher flow, which was due to a higher rate of cement grain dispersion provided by the superplasticizer admixture. SHC demonstrated a significant potential of crystalline admixture to recover the mechanical strength, regardless of the cement content. Even with the crack induction applied at 7 days, SHC developed compressive and tensile strength values with low differences of the reference concrete considering the same cement consumption and age (28 or 90 days). Regardless of the cement content, the crystalline admixture showed to provide a more evident decrease in the capillary water absorption and also in water penetration depth from 28 to 90 days, which indicated changes in the internal pore network. The effect of crystalline admixture in porosity was more evident at 90 days

and in concretes with higher cement contents, where there was a considerable reduction of water absorption and void index. Data obtained indicated that the cement consumption, when used in content higher than 450 kg/m3, was not a crucial factor in the mechanical strength recovery of a pre-cracked SHC. However, the increase in cement content showed to be beneficial to obtain a more accentuated reduction in porosity and pores connections of SHC.

ACKNOWLEDGEMENTS

The authors acknowledge the Coordination for the Improvement of Higher Education Personnel (CAPES) - Finance Code 001, PIC-FACENS, and the National Council for Scientific and Technological Development (CNPq) for financial support. LEMAT-FACENS is thankful for technical support.

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