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Different Setting Time

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Different Setting Time

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Contents lists available at ScienceDirect Construction and Building Materials ELSEVIER journal homepage: www.clsevier.com/locate/conbuildmat Effect of temperature on geopolymer and Portland cement composites modified with Micro-encapsulated Phase Change materials ar Shima Pilehvar*, Susana G. Sanfelix*”, Anna M. Szczotok’, Juan Francisco Rodriguez‘, Luca Valentini“, Marcos Lanzén*, Ramén Pamies', Anna-Lena Kjoniksen ** Hoc of Egicering aol Universi Clee PO. Bae 700, 1757 Helden. Norway * epartanente de Quin orgie nies de Malaga, Campus Terns sn. 29071 Malaga, Spain “Departmen of Chena Engineering Univesity of Csi = La Manca, 15004 Cad Real Spa “Deparoent of Geoscience Univer of Pod, 5131 Pa. ay “Departament de Argutecury Teel dee Eicon sues Tec Spe de AgutectrayEcecén ETA, Universidad Pode de Cartagena 30205 Aso 52: Cartagena Span “eperameot de Inger Mecca Materiales yFabceén Universe Polen de Cartagena, Cope. Murcia, pen HIGHLIGHTS + Micrcapsules slow down the reaction ofboth geopolymer and Portland cement pastes. “increasing the temperatute accelerates the siting times of geopolymer and Portland cement pastes {Addition of microcapsules reduces the compressive strength {Enhanced porosity at higher temperatures for bath geapolymer and Portland cement ARTICLE INFO ABSTRACT ‘rice iy Received in revised form 39 Mach 2520 ‘Accepted Api 2020; ‘To reduce pollution and global warming, the energy consumption needs to be decreased incorporation of Phase Change Materials (PCM) into bulding materials can help lower the energy needed to cool and ‘warm buildings. while keeping the indoor temperature ata confortable level, However, incorporate ‘of PCM into consritton materials alter their performance. In this study, the effect of temperature And addition of two different Microrencapsulated Phase Change Materels (MPCM) to zeopolymet ‘onesete (GPC) and Portland cement concrete (PCC) and pastes was investigated. The samples were Kom sscthuechnettamay amined ih blow (20°C) ant ave 80°) the meng pi te ea. Whe te MFCM Perland cement ve hot damaged by the alkaline solution, & few microcapsules are broken during the mixing process Coe Cea clnesy shows tha MPCML in sows own te Teton rate of bah eeopeyet and Portand cement paste. The setting times were faster when the temperature was incteased. The mechanical properties are reduced when MPM is added t0 GPC and PCC, although the compressive stength s adequate for building appcatons. Microstructural stuges show mote uniform and nda ged edges inthe shell-concrete matrix transition zone of GPC than PCC, The samples cured at 40 °C ‘exhibits more ar voids in both GPC and PCC than at 20°. '9 2020 The Author(s}, Published by Elsevier Le. Ths isan open access article under the CC BY Hcense (htplfreativecommons orgicensesiby/40). Compresive sength Ithermal arity 1. Introduction tion is an exothermic reaction that involves dissolution of silico aluminates in an alkaline solution and provides an amorphous 10 ‘The production of Portland cement is a major contributor to CO> ‘emissions [1], One of the efforts to reduce the CO; produced by concrete is to develop geopolymer-based building materials, con- sisting of inorganic alumino-silicate polymers |2), Geopolymeriza- responding author [mal eres sn ijonivenshiotne (AL. Kents) oso org)10.1016) cnbusémat2020 119088, 0830-0618 2020 The Authors) Pulse by sever ie semicrystalline three-dimensional network (3). The aluminosi- ‘ate sources can be natural minerals, like kaolinite, metakaolin and clays [24] oF industrial secondary products such as fly ash (FA), ground granulated blast furnace slag (GGBFS), red mud, and silica fume [5-7], Sodium hydroxide (NaOH), sodium silicate (a,Si0,). potassium hydroxide (KOH), and potassium silicate (K,Si0;) are commonly used as the alkaline solutions. Generally. geopolymer concrete (GPC) exhibits improved mechanical 2 5. lear et al Constrained Buling Materia 252 (2020) 18055, performance in comparison with conventional Portland cement conerete (PCC) [8.9 Buildings accounts for approximately 1/3 of the global energy demand and about 30% of CO, emissions, and more than 50% of the energy use of buildings is heating and cooling [10]. Accord ingly, obtaining new building materials containing Phase Change Materials (PCMs) is attracting interest, to reduce the energy consumption while retaining comfortable indoor temperatures [11-13], PCMS are compounds that absorb, store and release ‘energy during the phase change within a specific temperature range. When the temperature of the environment rises above the ‘melting point of the PCMSs, the PCMs absorb heat while changing ‘rom solid to liquid. When the temperature decreases below the ‘melting point of the PCMS, the heat of fusion is released back to ‘the environment and the PCMs return to a solid state 14), In hot climates such as southern Europe, PCMs prevent buildings from ovesheating at daytime during the warm season, and may also attenuate the necessity for heating at night during the cold months [15-18], PCMs with melting points in the range of 10 to 30 °C should be used to facilitate humman thermal comfort 19). Microen- capsulation of PCMSs is conducted to avoid interactions between the PCMs and the surrounding environment, to provide a high heat transfer area, and to prevent leakage of the core material during. the phase change [20 Im order to obtain new structural materials with improved ther- mal energy storage, Micro-encapsulated Phase Change Materials (MPCM) have been incorporated in concrete (21,22). However, the mechanical properties of concrete are diminished with the addition of MPCM [23-26]. Despite reduced concrete compressive ‘strength after adding MPCM, the compressive strengths are mainly ‘within the desired range (25 to 40 MPa) suitable for constructional purposes [27) Studies of the mechanical strength of geopolymer (25.28.29) and Portland cement (21,25,30] composites with incorporated MPCM have been reported previously. In addition, their ability to ‘enhance the thermal properties of the building materials for reduc~ ing the energy needed to keep a comfortable indoor temperature hnas been explored [31-35]. However, there are few previous stud ies utilizing isothermal calorimetry to examine the influence of the addition of MPCM on the reaction kinetics of Portland cement [36.37], and such studies of geopolymers seems to be lacking The aim of ths study is to evaluate how incorporation of diffe ‘ent types of MPCMs, above and below the melting point of each PCM influences the reaction rates, physical and mechanical proper- ties and the microstructure of both geopolymer and Portland ‘cement composites. Ths isa contintation of our previous studies [25,38,39], where the effect of MPCMs on the slump, setting times, ‘microstructure, mechanical stcength, and the effect of freeze-thaw cycles had been studied. We have also previously examined rheo- logical properties of pre-set Portland cement and geopolymer pastes containing MPCM (40,41), and the thermal properties of PCC and GPC containing MPCM [21-35] Unlike the previous stud- ies, this paper focuses on how MPCM addition affect the reaction kinetics of the samples, utilizing isothermal calorimetry at both 20 and 40°C. In order to gain additional information, setting times ‘and compressive strengths are examined at the same tempera ‘ures, and finaly scanning electron microscopy (SEM) and X-ray tomography were usilized to explore how the microstructure of the samples were affected by MPCM addition at these conditions ‘Two different MPCMs were compared: PE-EVA-PCM has an amphi Philic polymer shell of low-density polyethylene (50 wes) and ‘ethylvinylacetate (50 WE), while St-DVB-PCM has a hydrophobic polymer shell of styrene (50 wt) and divinylbenzene (50 wt) Both MPCMs have a paraffin core, with slightly diferent melting points 2. Materials and methods 2.1, Materials In order to prepare geopolymer composites, an alkaline activa tor solution, class F fly ash (FA), ground granulated blast furnace slag (GGBFS), sand, and gravel were used. The alkaline solution consisted of sodium hydroxide pellets and sodium silicate solution (25 w1% solid) A poly-naphthalene sulfonate polymer (FLUBE OS 439) was used a¢ 2 superplasticizing admixture to improve the workability of GPC and decrease the amount of water. Portland ‘cement I mixed with FA was used for Portland cement composites preparation. Dynamon SR-N, which is a high-performance super- plasticizing admixture based on modified acrylic polymers, was utilized to improve the workability of PCC. The densities and sup- pliers ofthe utilized materials are shown in Table 1, The composi- tion of the fly ash class F (FA) is 50.83 wt SiO,, 23.15 wt Al, and 6.873 wt CaO, The ground granulated blast fumace slag. (CCBES) consists of 34:51 w0t SiO,, 103 wt% ALO, and 42.84 wt % C20. Portland cement Il (Blaine fineness of 4500 em"/g) was pre-mixed mixed with FA from the supplier Im this study, two different MPCMs denoted PE-EVA-PCM and St-DVB-PCM were utilized. The synthesis of these microcapsules is described in previous publications [42.43]. The properties of the MPCMs are summarized in Table 2, St-DVB:PCM has a hydrophobic shell, while the shell of PE-EVA-PCM is amphiphilic (both hydrophilic and hydrophobic groups). The workability of the pre-set samples becomes poorer with the addition of MPCM [28]. Enhanced hydrophobicity of the MPCM shell reduces amount of water adsorbed onto the microcapsules [38.40], s0 that Tess water is needed to obtain a good workability 38,40,41]. PCMs with melting points around 28 °C and 24°C were chosen, since this {is within the range considered optimal in cooling dominant el- mates [44] In order to distinguish the differences in shape and size of the ‘components, SEM images of fly ash, slag, cement, and the two ifferent kinds of microcapsules are provided in Fig. 1. While PE-EVA-PCM reveals a cluster structure due to a high amount of agglomerates. a spherical shape is observed for StDVB-PCM [26.34], The PE-EVA-PCM clusters are mainly due to non- encapsulated PCMS [45] 22. Specimen preparation ‘An alkaline solution consisting of a mixture ofa sodium silicate solution (35 w0 solids, from VWR, Norway) and 14 M NaOH(2q) (prepared from sodium hydroxide pellets, from VWR, Norway) at 2 ratio of 15 was used for all geopolymer samples (38). The rable? round granultee bast 285 Cemex Germany ‘when sand 2.70 Canna Hath AS, Norway Sodium nyvende pellets 213 a Norway Sodium sitcatesoisen 193 we Norway (3s we sold Dynan St 110 MATE Neway 5; lear et al /Consraction an uling Mati 252 (2020) 119055, 2 able Propet of the we MFCM 243) Properier TERA SOV Shel composi Tow densi paetilene [30 wis) styrene (50 wi) ‘ybinylaceate (50 wt) Davbencene (sows) core mater Partin Pecan Meting point 264209: piazos'c renter SRA iE 2) Se. ie alkaline solution was prepared 1 day in advance to ensure com- plete dissolution of NaOH pellets and to lose the exothermic reac- tion heat. The microcapsules were added to the paste and concrete by the MPCM additive method and the MPCM replacement method. respectively [26]. The MPCM is added as an extra additive (Gn volume} to the powder materials in the additive method [46 In the replacement method, a certain percentage of sand (in volume} is replaced with the same percentage of MPCM [45], The replace- ‘ment method cannot be used forthe pastes, since they do not con- tain any sané. 22.1, Paste preparation For geopolymer paste, the alkaline solution and geopolymer binder (Fy ash + slag) was utilized at a ratio of 04. For Portland ‘cement paste, a fixed water to cement ratio of 0.35 was used. In the case of the isothermal conduction calorimetry, the materials containing the MPCM were weighed in the calorimeter glass ampoules and loaded into the isothermal conduction calorimeter ‘channels without mixing. In the setting times measurements, the ‘geopolymer binder and alkaline solution (for geapolymer paste) and cement and water (for Portland cement paste) were mixed for 90 5. Ater the subsequent addition of the microcapsules, the samples were mixed for another 90 s, resulting in homogenous pastes with the same consistencies 2.22. Concrete preparation ‘The ratio between the liquid (alkaline solution + extra water) and the geopolymer binder, as well as the water to cement ratio ‘of Portland cement were both kept atthe same value of 0.5, Addi tionally, the total amount of sand and gravel for the concrete sam— ples not containing MPCM was approximately the same for GPC and PCC. More details regarding the sample preparation can be found in Pilehvar ef al. [26.58]. The amount of MPCM in the sam- ples were chosen based on previous studies [25.24.35.38], with the aim of maximizing the thermal storage capacity while keeping ‘the workability ofthe pre-set samples and the mechanical strength of the concrete within an acceptable range. The components of the Portland cement and geopolymer mixtures are shown in Table 2 and Table 4, respectively. 223. Casting and caring GPC and PCC where 0 and 20% of the sand was replaced by MPCM, were cast into 10 x 10 x 10 cm? molds: see Pilehvar ‘etal, [26] for details. After a 24h precuring period at room temper~ ature with 2 90% relative humidity, both GPC and PCC samples ‘were demolded and cured in water at 20 or 40°C (below and above ‘the melting point of both MPCMs) for 1, 7, 14. and 28 days. 23, Testing methods 23.1. MPCM shel resistance against alkane solution and mixing process “To determine the resistance of the MPCM shell against the strong basic environment of the alkaline solution, St-DVB-PCM. ‘was immersed in alkaline solution for 7 days. EDX mapping and ‘SEM images of St-DVB-PCM alter immersion were performed by scanning electron microscopy (SEM), Hitachi $3500N microscope. ‘Additionally, SEM images of St-DVB-PCM after mixing with aggre- gates and water for 3 min were utilized to explore whether the ‘mixing process affects the shell of the micracapsules. Tis experi- ‘ment was only conducted on St-DVB-PCM, since the irregular ve 2/ F PEEVAPCM 100 ym_ MAG: 500s MAG: 5005 SEDVE-PCM 100 un, ig. 1. SEM images f(a thy sh (b) Sag.) Foca een (8) PEEVA.PCM ane) S-OVB.PCM 4 5. lear et al Constr and ulding Materia 2522020} 18055, Table Composvan of he geome composes. Werle Tae Cone) Compostian of he Poland cement compass Woerale Fase ‘onetete igh shape of PE-EVA-PCM (Fig. 1d) makes it difficult to distinguish ‘whether the shell is damaged during the mixing process 232, othermal conduction calorimetry The effect of different MPCMs on the heat evolution of the geopolymer and hydration reactions was studied in an eight- channel isothermal conduction calorimeter (TAM Air instrument) using Admix glass ampoules. All materials were mixed inside the calorimeter channels, after equilibrating them within the calorime- ter at the measuring temperature for 24 h. The calorimetry was conducted on geopolymer and Portland cement pastes containing (0% and 20% MPCM. The heat flow was collected for 3 days from the start of the reaction at both 20 °C and 40 “C. As mentioned in ‘in section 2.2, the MPCM is added as an extra additive (in volume) to the fixed binder mass (additive method). 233. Setting time ‘A computer controlled Vicat needle apparatus (ToniSET One, ‘Model 7301) was utilized to measure the initial and final setting ‘times in accordance with EN 196-3, The measurements were per= ormed on geopolymer and Portland cement pastes without micro- capsules and containing 20% MPCM at both 20 °C and 40 °C. In ‘order to measure the setting times at 40 °C, the basin was filled with water and the conical mold containing the paste was kept inside this basin, which was kept at 40 °C by water circulation through a thermal bath allowing temperature control (£0.1 °C), The setting times was measured at intervals of 2 min and 10 min for geopolymer paste and Portland cement paste, respectively The intial setting time was defined as when the needle penetra- tion is less than 39.5 mm, and the final setting time at a penetra~ tion of 05 mam, 23.4, Compressive strength The compressive sirength was measured at 40 °C by thermally insulating the compressive strength machine and connecting i to «aheating chamber. The compressive strength tests were performed in accordance with EN 12390-3. To remove excess water before initiating the measurements, the cubes cused at 40 °C were kept in a heating chamber at 40 “C for 1 h before being weighed and tested. Three cubes were used for each sample to obtain the reported averages. For comparison plirpases, measurements were also caried out at 20 °C. 235, Microstructural studies Scanning electron microscopy (SEM) (Hitachi $3500N) was used {in order to analyze the morphology of the fracture surface of GPC and PCC specimens without MPCM and with 20% St-DVB-PCM or PE-EVA-PCM cued at 40 °C. The SEM images were captured at 15 KV using back scattered electrons (BSE) to improve the exami- nation of chemical differences on the samples surface. ‘The internal visualization of the specimens was performed by X-ray tomographic scans, The measurements were conducted by a Bruker Skyscan 1172 CT scanner utilizing 85 KV incident radia- ton, a rotation step of 03°, and 600 ms exposure time per frame, The measurements were performed on cylindrical samples (1 cm height and 1 em diameters) of PCC and GPC without microcapsules and with 20% MPCM cured at 40°. 43. Results and discussion 3.1, MPCM shel resistance against alkaline solution and mixing process EDX mapping and SEM images of St-DVB-PCM after immersion in the alkaline solution are presented at two different magnifica- tions ih Fig. 2a and b. As previously abserved for other types of ‘microcapsules [47]. the MPCM are resistant to the alkaline solution since no broken or damaged particles are observed in Fig. 2. In addition, the capsules sutlace is mostly displayed in blue (color assigned to Cin Mapping) suggesting thatthe shell daes not retain Significant amounts of alkaline solution due to the hydrophobic nature of the shell. Additionally, MPCMs are clearly surrounded by a Na-rich phase. High NaOH concentration in che alkaline solu- ton might cause Na;CO; formation (by carbonation due to atma- spheric C0,). SEM images of St-DVB-PCM after mixing with aggregates and ‘water for 3 min is shown in Fig. 3, to scrutinize whether the mixing. process affect the shell of the microcapsules. It is evident that the ‘mixing process can cause ruptures on the microcapsule shell. A broken MPCM and possible surface damage can be seen in Fig. 2a 5 leva tl Corti end uling Meters 2522020) 18055, Allaline solution/ St-DVB-PCM MAG: 90x Alkaline solution/ St-DVB-PCM MAG: 500x Fig 2) EOX a ster of -D¥B-FCM immerse in alkaline sluin (b) SEM image of single arte of S-DVIAPOM fer immetsng in allaline solution fo 7 ays St-DVB-PCM after mixing __40 um __ MAG: 900x | SeOvE-PCM after mixing StOVB-PCM after mixing MAG: 700% ig. SEM images ef the SeDVE-FCM ster ning a) magiction of 006 at a magneton of OOK (the ae sows pat surface damage ofthe shel). and) sats magnicton of 9x (te arows sow that Some microcapsules are Broke and b, respectively. However, from Fig. 3c, with a wider field of ‘view, itis clear that only a few microcapsules are broken or dam- aged ding the mixing process. The MPCMs have less stifiness and strength than the aggregates. This might cause deformation and ‘Fracture ofthe MPCM during mixing. which will concribute 0 low= ‘ering the compressive strength of concrete [26) It shoul be noted that the field of view is limited, and it is therefore dificult to est- mate the percentage of broken MPCM. The itregular shape of PE- EVA-PCM makes it dificult to distinguish between damaged and undamaged shells These experiments were therefore conducted only on St-DVB-PCM microcapsules. 3.2 Isothermal conduction calorimetry ‘The rate of reactions in geopolymer anc Portiand cement pastes, ‘without MPCM and with 20% of t-DVB-PCM and PE-EVA-PCM was studied by isothermal conduction calorimetry. In order to evaluate ifthe reactions are affected by whether the PCMSs are in a solid ot liquid state, experiments were conducted at 20 °C and 40 °C for 72 h. For geopolymer paste, the frst peak in Fig. 4a has been reported to be related to wetting and dissolution of FA and GGBFS 51). Comparison with sheological data on similar geopolymer pastes Suggest that geopolymer precursors (monomers) are also ‘ 5; lear et al Constrained ling Materia 2522020} 18055, 03 Reaction ime (hou) ‘47 pamafoe z i277 fate” Fo" 2k pecevaeou 3 Sorte necasas.| Bag [ec so Be Sea é co z cecsayreenten | 5 otc = 6. raion fe if i 2 2 ° ° as 1 7 to GGT Otto t00 Reaction tme (haut) Fig 4 Heat Bow versus tection ine fra) geopelymer paste and (b)Fortang cement pst otmed at this stage [40]. The shoulder observed at longer times is 4 second peak, which overlaps withthe first peak This second peak is due to the geopolymerization reaction [40°51], As can be seen. from Fig. 4a, geopolymer dissolution and formation of geopolymer precursors starts within the first 10 min after mixing materials at ‘both 20 °C and 40 °C, However, the heat evolution peak at 40 °C ‘was higher in this step since more FA and GGBFS can dissolve at high temperatures. Inerestingly, both the first and second peak are shifted towards longer times when the temperature of the -eopolymer paste is raised, even though higher temperatures is ‘expected to speed up reaction rates. This is probably because the dissolution step and the formation of geopolymer precursors can continue for a longer time at high temperatures (shifting the top ‘of the fist peak to longer times). The formation of more geopoly- ‘mer precursors enhances the viscosity of the samples. Accordingly, the transportation of the monomers is slowed down, and the 3D _geopolymer network takes longer to form | 40 shifting the second, peak to longer times) For Portland cement (Fig, 4b), there isa first peak related to dis- solution and early cement hydration followed by an induction per= jod before the main hydration peak at later times [52,53], The dormant induction period is commonly observed for Portland ‘cement, and thought to be related toa slow-down of the dissolu- tion process due to low undersaturation (52,53), The hydration process ofthe second peak reached its maximum value within 5~ ‘1h. As expected, increasing the temperature from 20 °C to 40°C accelerates the hydration reaction (54,55). However, there is a ‘eduction in heat flow at early ages (dissolution step). This is prob- ably due to 2 faster approach to low undersaturation at higher tem- peratures. The second peak is much higher at 40 °C, due to the ‘temperature-induced acceleration ofthe hydration reaction (54), When exposed to an aqueous environment, the microcapsules retain water. S-DVB-PCM adsorbs water corresponding to 45% of its weight, while PE-EVA-PCM adsorbs 65% due to the more polar nature of the microcapsule shells [38]. This affects the effective water content in the samples, which has a complex effect on the reaction kinetics. Less available water in a system will normally cause 2 viscosity increase (56-58). This has also been observed. for pre-set Portland cement paste [4) and concrete [26], as well as for pre-set geopolymer paste [40] and concrete [25,38]. Since the components will move slower at higher viscosities (Stokes- Einstein relationship), it will take a longer time for the reactants to encounter each other. Accordingly, a viscosity increase may slow down the reaction rates [38]. On the other hand, a lower amount of available water will increase che effective concentration of the teactants, which may result in faster reaction rates [40]. ln addi tion, for the geopolymers the rate of aluminosilicate dissolution is expected (o increase when there is less water in the samples, ‘due fo the resulting higher concentration of OH" (59|, A higher OW" concentration might also speed up both the formation of sgeopolymer precursors and the polymerization of these precursors Into the geopolymer network, since both these reactions involves OH" as one of the reactants [40,50\61|, However, if the water retained by the microcapsules also includes the dissolved OF ions, the concentration of OH” would not be affected and this effect could be neglectable. At very low water conditions the geopolymer reaction rate is expected to decrease when the available water is reduced, due to stabilization ofthe anions which reduce the rate of the condensation reactions (59). A smaller water content will also lower the total amount of reactants that can be dissolved before the sample reaches saturation. Accordingly, low undersatu- tation will be approached faster, which may slow down the reac- tion. The different effects a reduced water content can have on the reaction rates is summatized in Table 5. The overall ellect of [MPCM addition (which decreases the available water) is expected to be 2 combination of these competing factors, and will depend ‘on which factor that dominates in each case, At 20 °C, MPCM addition to the geopolymer and Portland cement paste causes a decrease in the peak intensity ofthe first peak (Fig. 4), Significant amounts of water are retained by MPCM particles (28), especially by PE-EVA-PCM (which contain polar groups) Since the peak reduction is more pronounced for PE-EVA-PCM, this suggests that the peak reduction is related to the adsorbed water. Less available water in the samples will lead to a faster approach to low undersaturation for the Portland cement and to less water for wetting and dissolution of FA and {GGBES in the geopolymer. Ths is expected to result inthe observed reduced height of the first reaction peak ‘While the frst peak of the Portland cement stays more or less in the same place with the addition of MPCM, the frst peak of the -geopolymer samples are shifted towards longer times in the pres- The eet of decreased avalable water Incest] a decree 1) ection tee. the reaction tes Te ara nate Ivey low water content higher eecive OF" concentration - ence of microcapsules. A lower availability of water is expected to increase the viscosity of the samples (40), which can slow down the formation of geopolymer precursors |38,52-54), thereby caus- ing the observed shift of the fist peaks toward longer times with MPCM addition, Interestingly. at 40 °C both geopolymer and Portland cement containing 20% St-DVB-PCM have slightly higher heat evolution of the fist peak than the samples without MPCM, while utilizing 20% PE-EVA-PCM still causes a reduction of the peaks. The reduc- tion of the peak heights for PE-EVA-PCM is probably related to the high amount of adsorbed water (as discussed above). The rea- son for the higher frst peak in the presence of ST-DVE-PCM at 40 °Cis unclear, For geopolymers, the cumulative heat during this time period is lower for ST-DVB-PCM than for pure water (Fig 5). ‘Accordingly, the total dissolution and reactions are reduced due to the lower water content inthe presence of ST-DVB-PCM, while the peak becomes narrower and thereby higher (Fig. 4a). For Portland cement, the cumulative heat is initially higher for ST-DVB-PCM than in water (Fig. 5d), suggesting that early cement hydration is increased due to a higher concentration of reactants (Table 5), For the geopolymer paste (ig, 4), the second peak is not mark- edly affected by MPCM addition. However, the overlap with the first peak makes it dificult to distinguish whether there are small changes. Since this reaction releases water instead of consuming t [65], tis less influenced by the available water in the sample (ex- cept for very low water contents (59]) The second peak of Portland cement paste (Fig. 4b) is shifted toward longer times when MPCM is added to the samples. This prologation of the dormant induction period is probably due to the water retained by the MPCM [38], which reduces the available water in the sample and thereby extend the period of low uundetsaturation, ‘As can be seen in Fig. 5a and c, there isa sharp increase inthe cumulative heat immediately after starting the geopolymerization, which corresponds to the first peak of Fig. 42, The total cumulative heat developed during the geopolymerization reaction is much higher at 40 °C than at 20 °C (Fig 5a) The elevated temperature speeds up the alkaline activation ofthe geopolymer binder, causing, ‘the final products to form faster [65]. ince the reaction does not seem to be completed within the timeframe of the experiments, this causes a higher cumulative heat at 40 °C. At 20 °C. the MPCM. is not significantly affecting the total amount of cumtlative heat developed during the reaction, However, at 40 “C the sample con- taining St-DVB-PCM has the highest cumulative heat at long times while PE-EVA-PCM has the lowest, The reduced cumulative heat of PE-EVA-PCM is due to the lower amount of available water, caus- ing higher viscosities and fewer reactants dissolved at saturation, This will slow down the reaction rates (Table 5), ané thereby result in lower accurnulated heat. The higher cumulative heat at long, times for geopolymets containing St-DVB-PCM at 40 °C (Fig. Sa) is not evident at short times (Fig. Se). This effect is therefore due to reactions occurring relatively late in the process. ie. when the geopolymer precursors ate combining into the 3D-geopolymer structure. Higher cumulative heat in the presence of St-DVB-PCM. at 40 °C occurs only after the sample has set (Fig. Ga), and the vis Cosities are therefore not the dominating factor. It is possible that the reduced water content increases the effective concentration of OH" in the sample [59], and that this speeds up the reaction ‘between the geopolymer precursors and OH" te form the geopoly~ mer network For Portland cement paste (Fig. Sb and there is a small upturn of the cumulative heat at short times, corresponding £0 the frst peak. This is followed by a period of slow increase (the dormant induction period) and a sharper upturn (the second peak) at longer times. As for the geopolymer paste, the total ‘cumulative heat is higher at 40 °C than at 20 °C. The addition ‘of microcapsules decreases the total accumulated heat at long times for both themperatures, This is probably caused by the as0 |e) pow = 0 eon Soo] |r 2 Soercevarcd : 2S dom Sioveeon 3 00 2 100 5 0 eopolymer sate 5 ater pas 0 70 20 30 40 60 Reaction time (hour) 6070 ja ‘Geopalyner paste Cummulative heat 250] (b) 200 Portland cement paste| 20 30 40 80 60 70 Reaction time (hou) 0% (@) Portane cement paste 04 2 3 Reaction me (hour) a 2 3 Reaction tine (hour) s 5. lear et al Constrained ulding Materia 2522020} 18055, ceopoymer paste 7 Donan cement poste 0 Be 8 a satra e s oo Ti Ft eugene Ee 2 <= es B 20 4 sea - ° 2 ig 6 The intl ang nal seing tes of (2) xopeimer pst and b Portland ement past cenaining 20 vs of PE-EVA-PCM and S-OVE-POM a 20 “Can 40°C adsorption of water onto the MPCM, which can reduce the Port land cement hyération. 3.3, Setting time The effect of MPCM and temperature on the initial and final set ting times of geopolymer paste and Portland cement paste is illus- trated in Fig. 6. As can be seen from Fig. 6a, the geopolymer reaction is significantly faster when the temperature is raised from 20 °C to 40 °C. As expected, the geopolymerization reaction is accelerated at higher temperatures without any significant effect ‘of MPCM addition. When the temperature increases, the solubility of aluminosilicate is higher. This results in larger quantities of alu- ‘mina and silica available for the geopolymerization reaction, speeding up the seting times of the geopolymer paste [67], Unlike the setting times at 20 °C (which is discussed previously (28), MPCM in liquid state (40°C) has no noticeable effect on the seting times, ig. 6b shows that a higher temperature (40 °C) leads to rapid hydration and shorter setting times for Portland cement paste than ‘at 20 °C [68]. At 20 °C, the initial setting time of Portland cement paste becomes longer in the presence of microcapsules due t0 the higher viscosity of the paste which leads to slower cement hydration [99), However, at 40 °C MPCM addition has no signifi- cant effect on the initial setting time of cement. After the initial setting time, the solidification of the samples becomes faster in the presence of microcapsules. due to the water adsorption on the microcapsules surface [38]. For the final setting time at both, 20 °C and 40 °C, the influence of PE-EVA-PCM is stronger than for St-DVB-PCM, since PE-EVA-PCM adsorbs higher amounts of water and has a smaller siamp (38) 34, Compressive strength The effects of temperature and MPCM addition on the compres~ sive strength and compressive strength reduction of GPC and PCC are shown in Fig. 7. As observed previously [26], GPC has a higher ‘compressive strength than PCC at both temperatures, In addition, the compressive strength of both GPC and PCC increase with curing, time and temperature, For GPC, the higher temperature speeds up the formation of a hard structure, especially in the early-stage of ‘the geopolymerization reaction (70), Analogously, the faster hydra- tion reaction increases the strength of PCC at elevated tempera tures. At early curing times, the increase of the strength with temperature is mare pronounced for the geopolymers, since the -geopolymerization is faster than hydration at higher temperatures (ig. 5) The 28-day compressive strength (Fig. 7c, d) decreases with the addition of MPCM [26), and increases with temperature. In addi- lerPce ah 40 0 Compressive strength (MPa) oF «0 w 0 Tf wm a Caring tine (ay) Curing ine (ay) F of PC a a 7 Efron |] Pocaay2s | Foo | 3 40 | 5 20. 6 : 0 2 PCM o (oy PCM (i) zg [eee [weet 5 are : ‘2 hou MECN & PE-EVApcM 8 2 subvaPoM ot «0 wo 7 wm a Curing time (ay) Curing time (day) IMCM, compressive srength of GPC and PCC a a fnction of the amount of sand replaced by MPM afer 28 ayy caring for (c) GPC, and (e) FCC Reduction of Cnnpesive strength du to MFCM addin fot e) GP with 20" MECM and (9 PCC sh 20 Men ‘ion, itis smaller for PE-EVA-PCM than for St-DVB-PCM, except for 20% MPCM for PCC at 20 °C, PE-EVA-PCM has an irregular shell and form agglomerates, which may enhance the compressive strength reduction. In addition, we have previously demonstrated that more air is trapped within the PE-EVA-PCM samples, due to 4 reduced workability [38]. This lowers the compressive strength 5; lear et al /Costractin an ung Mati 252 (2020) 119055, . GPC 20% PE-EVA-PCM — MAG:900x GPC 20% St-DVB-PCM MAG:500x Fig 8. SEN images of he rac PCC 20% PE-EVA-PCM PCC 20% St-DVB-PCM, MAG:S00x src ofa) GPC conning 20% E-LVA-PCM.(b) PCC containing 20% E-LVA-HCME (c) GC containing 20% S-DVE-POM, anf PCC ‘anaining 202 S-DVD-PCM The rows show the edge of shellconrete mats tanion Yon, in comparison with St-DVB-PCM. Furthermore, PE-EVA-PCM con- tains significant amounts of non-encapsulated PCM [45], which right reduce the strength ofthe concrete. The reduction of GPC and PCC compressive strength in the pres- ‘ence of 20% PE-EVA-PCM and St-DVB-PCM are shown in Fis. 7e and F. When cured at 20 °C, GPC has a stronger strength reduction at short curing times, However, after about 1 week it stabilizes at an approximately constant value. When cured at 40 °C. the reduc- tion of GPC strength is almost constant at all curing ages. At long times, the strength reduction is approximately the same for the ‘GPC samples cured at 20 and 40 °C, which is probably caused by the faster geopolymerization at higher temperatures (Fig 5). The reduction of GPC strength is more pronounced for samples con- taining PE-EVA-PCM than for St-DVE-PCM. PCC containing PE- EVA-PCM and St-DVB-PCM show approximately the same strength reduction at 20 °C, However, for PCC cured at 40 °C the strength reduction is much higher in the presence of PE-FVA-PCM than for St-DVB-PCM. Melting the core ofthe microcapsules i expected to make them mechanically weaker, and therefore deteriorate the ‘concrete strength. Interestingly, for PCC containing St-DVB-PCM, the strength reduction is significantly lower at 40 °C than at 20°C (Fig. 1. This is probably caused by the higher mechanical strength of PCC cured at 40°C (Fig. 7b), which makes it ess vulner~ able to softer particles. Comparing the temperature effects of the Strength reductions of PCC and GPC, PCC is more affected by increasing the temperature above the melting point of the MPCM core than GPC. A more uniform and compact structure of GPC together with its initially higher mechanical strength may con- tribute to a better resistance against the softening ofthe particles. 3.5, Microstructural analysis 3.5.1, SEM imaging SEM analysis was conducted on the failure surface of PCC and ‘GPC samples containing 20% St-DVB-PCM and PE-EVA-PCM cured, at 40 °C, Fig. 8 shows individual particles of St-DVB-PCM and PE- -EVA-PCM in the GPC and PCC matrixes as an example of how the (MPCMs shell binds with the surrounding matrix Fig. 8 illustrates ‘that there are more uniform and undamaged edges in the shell- conerete matrix transition zone of GPC than PCC. This illustrates 4 better compatiblity between the MPCMs shell with GPC than {or PCC. This might contribute to a better performance of GPC than PCC in the presence of MPCMs when the samples are exposed to temperature fluctuations from 20 “C to 40 °C oF vice versa (Fig, 7a and b) Smaller gaps are observed atthe interface between St-DVB-PCM and the concrete matrix compared to PF-EVA-PCM, suggesting a better compatibility between the St-DVB-PCM shells and the sur= rounding matrix. The larger gaps combined with agglomeration of PE-EVA-PCM and non-encapsulated PCMs in the PE- EVA-PCM samples [45] contributes to the greater reduction of E-EVA-PCM compressive strength compared to St-DVB-PCM 35.2. X-ray micro-tomograpiy ‘Typical 20 X-ray micto-tomography cross-sectional slices of {GPC and PCC without MPCMs cured at 20°C and 40 °Cate depicted in ig. 6. To obtain reliable statistical data, more than 600 2D slices ‘were taken foreach sample. As seen in fig 9a and b, more ait voids are visible inthe GPC samples cured at 40 °C than at 20°C. Increas~ o 5: lear et al Constrained ulin Materia 2522020} 18055, Gece tomography unages of (2) GPC without MECM at 20 °, (0) GPC Mechta 40° (6) 2 tout MPCM 320 and 4) PCC hou MPC [E40 'C Dat alr niet lon no abrorpion of ray [eg merospeles oF {ie bie} and bight ots inate igh absorption ef aps gavel abd sae) Se mages have approximately 1 er ldo ew ing the curing temperature is known to dissolve more Si and Al {rom the amorphous phases. This accelerates the development of hard structure, especially during the inital stages of the geopoly- ‘merization reaction. Accordingly, higher temperature increases water evaporation rates thereby producing further air voids (72 This causes the formation of micro-cavities, and therefore an increase inthe porosity ofthe GPC matrix. For PCC, higher temper= atures enhance the hydration rates This results in a more hetero ‘geneous hydration distribution, and enhanced porosity, Lower temperatures results in a more homogenous and uniform distribu- tion of the hydrates, and thereby the formation of smaller pores ia ¢. 10 shows the distribution ofthe MPCMSsin the GPC ané PCC matrix. Given the low level of X-ray attenuation of the MPCMSs, itis challenging to utilize grey scale values to distinguish between air voids and microcapsules. However, since air voids tend to be spherical, irregular profiles are probably due to agglomerated MPCM. Fig. 10 shows that both agglomerated St-DVB-PCM and PE-EVA-PCM are distributed throughout the PCC samples. GPC has some regions containing agglomerated MPCMs and some more homogeneous regions without any MPCMs distribution. The ‘enhanced viscosity (reéced workability) of the fresh GPC and the fast setting times of GPC especially at 40 °C can contribute t0 the prevention of a homogeneous distribution of MPCM through- ‘out the matrix, 4. Conclusion Incorporation of PCMs in building materials can help reduce the ‘energy needed to heat and cool buildings, while retaining a com- {ottable indoor temperature. However, inclusion of PCMs in con- struction materials influence many aspects of their performance In this paper, the influence of two different MPCMs in liquid and solid state (above and below the melting point of the PCM core) ‘on the reaction kinetics, physical, mechanical and microstructural * Sere rete seers eee Teens eee (eats seme {ontaning 20% S-DVB-PCM at 40°C Dak clos indicae low oF no absorpion of properties of Portland cement and geopolymer concrete(pastes Were investigated. The following conclusions can be drawn from this work 1, The mierocapsuies shell can resist the highly basic nature of the alkaline solution without any leakage or damage, A few micro- capsules were broken and damaged during the mixing process due tothe lower stifiness and strength ofthe MPCM shell com- pared to the conventional aggregates. 2, Isothermal calorimetry shows that MPCM addition slows down, the reaction of both geopolymer and Portland cement paste at 20°C, which is probably due to the water adsorption onto the ‘microcapsules. At 40 “C, the effect of microcapsule addition is ‘more complex, and St-DVB-PCM are speeding up some of the 3, The setting times of geopolymer paste and Portland cement paste were accelerated at higher temperatures due to faster geopolymerization and hydration. MPCM in liquid state (40°C) has no noticeable effect on the setting times of geopoly- mer paste. For Portland cement paste, PE-EVA-PCM as a greater influence on the final setting time than St-DVB-PCM, since much mote water ate adsorbed onto PE-EVA-PCM, 4, The compressive strength of both GPC and PCC increased with curing time and temperature. However, MPCMs addition reduced the compressive strength. and heating the samples above the melting point of the MPCM core affected PCC rmuch ‘more than GPC, The strength reduction was more pronounced for PE-EVA-PCM than for St-DVB-PCM. The irregular shel agglomeration, and reduced workability of PE-EVA-PCM are probably the major contributing factors for this. 5. A more uniform and compact structure of GPC combined with higher mechanical strength might contribute to the better tesis- ance against softer particles. These were mote uniform and undamaged edges in the shell-concrete matrix transition zone ff GPC than for PCC. This might contribute to the better perfor- 5; lear et al /Consraction an uling Mati 252 (2020) 119055, "0 mance of GPC than PCC when microcapsules are added to the ‘samples. Porosity was enhanced at higher temperatures in both GPC and PCC. Incteased viscosity (poorer workability) of the fresh GPC and the fast setting times of GPC especially at 40 °C may contribute to the prevention of 2 homogeneous distribu tion of MPCM throughout the matrix, ‘CRediT authorship contribution statement Shima Pilehvar; Conceptualization, Methodology, Validation, Investigation, Writing - original draft, Writing - review & editing ‘Susana 6, Sanfelix: Investigation, Writing - review & editing, Anna 'M. Szezotok: Investigation, Writing - review & editing. Juan Fran- ‘isco Rodriguez: Investigation, Waiting - review & editing. Luea Valentini: Investigation, Writing - review & editing, Visualization. ‘Marcos Lanz6n: Investigation, Writing - review & editing, Visual- ization, Ramén Pamies: Writing - review & editing, Visualization, ‘Supervision. Anna-Lena Kjaniksen: Resources, Writing - review & ‘editing, Visualization, Supervision, Project administration, Funding acquisition Declaration of Competing Interest ‘The authors declare that they have no known competing finan- cial interests or personal relationships that could have appeared to influence the work reported in this paper, Acknowledgement ‘We gratefully acknowledge funding from the Research Council ‘of Norway, project number 238198, The authors acknowledge Fun- «laci6n Seneca Agencia de Ciencia y Tecnologia de la Region de Murcia “Ayuda a las Unidades y Grupos de Excelencia Cientifica de la Region de Murcia (Programa Séneca 2014)" (Grant 19877/GERM/14), for financial support. References. IN] £ eabela, G. ahed & Shamsaet A. Bakador, Gibal [Bsns oper nn pec hew mata The A Is] [Davida Cepolynes Chemisty and Appiatons, astute Geopelynte, Suge-Quentia ance, 2011 Ia) Cit wp Co they, Pros, Js. an Deveney, fect f calcu sae Suices oa geoplymecsiten, Cen Cove es 3 4) (2008) 354-563 Is] ELDiar EN Alouche 5. Slund, Facots fein he sutabliy fy ash as [6] P- Nath PK. Sather, fect of GGBFS on setting, werkality and early strength properties of yas geopolyerconctce cee ambient cobitian, Const Bld ste 66 (20e4 63-171 [71 S-Thokehom, Daas. cos, Etec of incorpo J Cleaner Ped 31 [8] G5. Ku. YB. Lee, KT. Koh. YS. Chung. the mechanical properties of My ash- Dased geoolyne oneet wih laine activators, const? Sule Mater 47 IO]. Fu, L Gai, W. Yonggen. Freeze-thaw cycle test and éamage mechanics ‘motel of slka-actwate slg cnerete, contr mid. Maver 5 (7 (001), 110]. Urgevorsat. K Pcihenka Mt. Anal M stanie.E Onde, Labrina. Lele. Bes Practice Pls for Law Caron nergy Bling A Seenaio ‘nals lab! Beings Peformance Network Bape! (207) 1 M'Gtetalome M Mates, LE cers hi Femaner ype methods, [Sipea"A rear Renew Sutin Paegy Rew 53 016) 138-1075 tna] RM. Khoa MM. Tard A review ene Sonerton sy biling ‘pplicatans wih thermal storage by atnt est ng pave change mates, 1a] Vv ag uaa FE her staragenllings: A sae fa Res 114] T-C-ting,C-5 Poa, Use af phase change materials foc thermal energy storage 115]. Akebee, Nejc, MZA. Majid, MA. Wabld, FE Jomehzadel, L. Zeyna Fumie, JX Calas BR. Hughes, S.A Zak Aceview on phase change material (POM) or sustainable passive cooling in bulking envelopes, Renew. Sustain [16] SE Kalnas BF. Jel, Phase change materials and products applications. A state-of-the-art review and future research opp Energy Build. 94 (2013) 150-176 [17] Nhu. 2 Ma. 5, Wang Dynamic characteristics and energy performance of bldings using phase change materials: review. Energy Convers Manage 90 [18] A ce Gracia, LF Cabeza, Phase change materials and thermal energy storage 2 buildings, Enerey ané Buieings 103(Supplement,C) (2015) 414-418. [19] D. Zhou. CY. Zhae. Vian. Rewew on thermal energy saraze with phase shange materials (PEMs} in. building applications. Applied Energy 52 [ao] MA. Hawiader. MS. Usin, MM, Khin, Miroenespeulates PCM thermal nergy storage system. Appl Energy 41-2 (2003) 195-202, 1211 Adda Dr Cel} Ne Cae Eerie ne mi ‘Therm, Eng 64 (to2} (2014) 22-38, 12] LF Cabera, Casein Mc Nogués, M, Medrano, R Leppes, 0 Zubillaga, Use 392) 2007) 113-118, Ra1 A etede, Lan, & Mente © Cardo, Meanie! an heal (2a teams Pte Beas. lout, D. Noveshaue, St Mason containing phase change mate Energy Bulé 94 2015) 52-60 (251 Mage 4 ap Ends 1 Brouwer BT Te beh: of [26] 5: Mlenvar, VD. Coa, AML Seeo(ok L Valenti, D Salvlont ML Magist. R fncapsulated phase chaige tells, Cet. Conc Res. 109 (2017) 341-349, 27] SH. Kesmatia 8 Reso Wc. Fapatese, NF MacLeod, RJ McGrath Desi and Contol of Concrete Mintues, Seventh Canaan Edition, Cement ‘Associaton of Canada (2002) 153 (28) R Shadota, L zhang P. Ui, Experimental study of geepolymer mertar with Incorporated PCM, Constr Bull. Mater 84 (2015) 95-102 {a9} 2: Wang. H. Su, 5. Zhae, N. Zhao, Infuence of phase change material on ‘mechanical and thermal properties ef clay geopelymer mart, Constr. Bul. Mater 120 2016) 329-334, [30] H. Zhang. F Xing HZ Cui DZ. Chen. X. Ouyang, $~Z Xu, JoK. Wang, Y= Huang J-D_2ve, JN Tang, A novel phase-change cement composite fer thrial energy store: Fabrication. thermal and mechanital prepecties, Ap [31] VD. Cao, TO Bu. Ac. Kjoniksen, Thermal analysis of muller walls ‘onsainine geepoiyme: concrete and phase change mates for Duileing 1321, on Pa Sigs AM, Seceak TO BM Carona FF (331 Vb'Gae5 Pea €SaoBrinas AM Serote F0 B M, Caen) Spplietins, Sol Energy 178 (2018) 285-307, [24] VD, Goo, & Pilevar, C Salastringas. AM, Sreztok. JF. Redviguer, Mt [35] VD. Co, 5. Petar, c Salas-Bringas, AML zczotk L Valentini, M. Carmona, [HF Reiguer AL Rinses, iitence of microcapsule size and shel polity 35] X Pang WIC menee, V. Goel. Use of Microencapsulaced Phase-Change [Materials To Regulate the Temperature of Owl Cemeat, SPE-20826-PA 31 e015), (271 BA Young ¢. Fazone. 2 She, AM. Thiele. Z Wel, N. Neitalth ©. Sant L Pon Eaiyage temperature evolutions in concrete pavements containing Ijcoencapsulated phase change materials, Const. Bul. Mel. 147 (2017) [58] 5 Plevar, VD. cao, AM, szcetok. Mt, Carmona. L Valen M Lanzén,R Pamies AL Kemksen Phystal and mechanical properties fly ast and sag seopelymer concrete containing efferent types of mice-encapulatee phase Change materials, Const Bul. Mater 173 (2018) 25-38. [39] 5 filehvar A Seczotok|F Rodriguez Valentin. M Lanzén,R.Pamies, AL Kieniksen, Eifec of freeze-thaw cycies on the mechanical behavior of copolymer concrece and. Portland cement concrete containing micro- ‘neapsulte phase change mateils,Const. Build Mater 200 (2019) 94-103 buteng 2 'S. Revaret a /Conarscton and ang Material 252 (2020) 119055 (Mo) vd. ca, sPietva.C Saas-Seingas, AM, Seczoto, NBD. Do, HT Le. Me Caidon, JF Roerigues,A-t Kjenhse,teenee of Micocapale Size ab Shel Play on the Tne-Dependeat viscose of Ceopelyne Past, be Eg hens Rex 979) 2018) at -8Ho4, (any Sc. Sande 1 Sancacruz, AM Seczotok LM. Slloe AG. De a Tose A ‘onsen, ttet of mesoencapsuated phase change materials onthe ow Devi of cement composts Constr, Bald: Mater 2082019) 382-262, (aa) At bateguere. IL Valvetee. JF Roctguez AHL Buber. |) Cuil, Carona syathess and charaetzaton of microcapsules

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