Translucent self-healing cementitious materials using ...application of translucent materials,...

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Translucent self-healing cementitious materials using glass bers and superabsorbent polymers D. Snoeck * , J. Debo, N. De Belie Magnel-Vandepitte Laboratory, Department of Structural Engineering and Building Materials, Faculty of Engineering and Architecture, Ghent University, Tech Lane Ghent Science Park, Campus A, Technologiepark Zwijnaarde 60, B-9052, Gent, Belgium ARTICLE INFO Keywords: Translucency Self-healing Ductility Durability Strain-hardening cementitious composite Hydrogel ABSTRACT Glass bers possess the ability of transmitting light through the core of the ber. However, most of the current manufacturing techniques are time- and cost-inefcient, limiting the implementation of translucent cementitious materials. The use of bers increases the ductility of the cementitious matrix and limits the crack widths upon loading. This is advantageous in terms of autogenous healing. This healing can be further promoted by the use of superabsorbent polymers. The combination of translucency using glass bers with promoted self-healing prop- erties using superabsorbent polymers was therefore assessed using a direct-mixing technique. The mixture composition was optimized, the translucent property was available, multiple cracking was achieved, cracks were able to visually close and the mechanical properties were regained. This opens up opportunities for further application of translucent materials, showing self-healing properties. 1. Introduction Concrete is a material known for its high structural performance, but it has a limited tensile strength, resulting in crack formation during the lifespan of a concrete structure. Furthermore, the presence of cracks endangers the durability as intruding gases and/or uids will cause corrosion of possible present reinforcements, next to other degradation phenomena. As the concrete structure gradually deteriorates, repair should be done as quickly as possible. However, the damage may go unnoticed, repairs may be postponed, or in some cases repair is even not possible due to a lack of accessibility of the structure. Fortunately, con- crete has a passive healing capacity, e.g. autogenous healing. By the combination of four different healing mechanisms, the cracks in the cementitious material are able to close. The healing mechanisms are (1) the blockage of the cracks by impurities, (2) the swelling of calcium- silicate-hydrates at the crack walls, (3) the further hydration and pozzolanic activity of not yet reacted binder particles, and (4) the cal- cium carbonate crystallization (Edvardsen, 1999; Granger et al., 2007; Snoeck and De Belie, 2019; Snoeck, 2018). Due to a decreasing amount of unhydrated particles as further hydration occurs in the system with time, the main healing mechanism at later ages will be the calcium carbonate crystallization (Snoeck and De Belie, 2019; Van Tittelboom et al., 2012). In order to take advantage of this self-healing feature, one needs to guarantee sufcient building blocks such as the availability of certain hydration products or unhydrated particles. On the other hand, a crack should be sufciently narrow in order for healing products to bridge the crack (Li et al., 2002; Li and Nawy, 2008). Additionally, water needs to be available to sustain the healing reactions (Snoeck et al., 2014a; Yang, 2008). In order to limit the crack width, bers may be added to the cementitious mixture. Multiple cracks with limited crack widths have been achieved using synthetic bers such as polyethylene (PE), poly- propylene (PP), and polyvinyl alcohol (PVA) bers (Li et al., 2002; Li and Nawy, 2008; Snoeck and De Belie, 2015a; Zollo, 1997; Li et al., 1997; Homma et al., 2009). These mixtures were optimized to have narrow cracks up to 3050 μm(Li and Nawy, 2008; Yang, 2008; Snoeck, 2015). This is a boundary condition for self-healing to efciently and completely close a crack even at later ages in this specic type of strain-hardening cementitious materials (Li and Nawy, 2008; Yang, 2008; Snoeck, 2015). Another possibility is the use of natural bers, such as ax or hemp, with or without chemical treatment to induce multiple cracking and a sufcient ductility (Snoeck et al., 2015a; Snoeck and De Belie, 2012). Both for natural and synthetic bers, the interaction between ber, cementitious matrix and ber-matrix interface leads to the wanted narrow crack widths. As the bers are evenly distributed in the cemen- titious matrix, the position of the cracks will be more evenly spaced in * Corresponding author. E-mail address: [email protected] (D. Snoeck). Contents lists available at ScienceDirect Developments in the Built Environment journal homepage: www.editorialmanager.com/dibe/default.aspx https://doi.org/10.1016/j.dibe.2020.100012 Received 16 April 2020; Received in revised form 14 May 2020; Accepted 14 May 2020 Available online 26 May 2020 2666-1659/© 2020 The Author(s). Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by- nc-nd/4.0/). Developments in the Built Environment 3 (2020) 100012

Transcript of Translucent self-healing cementitious materials using ...application of translucent materials,...

Page 1: Translucent self-healing cementitious materials using ...application of translucent materials, showing self-healing properties. 1. Introduction Concrete is a material known for its

Developments in the Built Environment 3 (2020) 100012

Contents lists available at ScienceDirect

Developments in the Built Environment

journal homepage: www.editorialmanager.com/dibe/default.aspx

Translucent self-healing cementitious materials using glass fibers andsuperabsorbent polymers

D. Snoeck *, J. Debo, N. De Belie

Magnel-Vandepitte Laboratory, Department of Structural Engineering and Building Materials, Faculty of Engineering and Architecture, Ghent University, Tech Lane GhentScience Park, Campus A, Technologiepark Zwijnaarde 60, B-9052, Gent, Belgium

A R T I C L E I N F O

Keywords:TranslucencySelf-healingDuctilityDurabilityStrain-hardening cementitious compositeHydrogel

* Corresponding author.E-mail address: [email protected] (D. Sno

https://doi.org/10.1016/j.dibe.2020.100012Received 16 April 2020; Received in revised formAvailable online 26 May 20202666-1659/© 2020 The Author(s). Published by Elsnc-nd/4.0/).

A B S T R A C T

Glass fibers possess the ability of transmitting light through the core of the fiber. However, most of the currentmanufacturing techniques are time- and cost-inefficient, limiting the implementation of translucent cementitiousmaterials. The use of fibers increases the ductility of the cementitious matrix and limits the crack widths uponloading. This is advantageous in terms of autogenous healing. This healing can be further promoted by the use ofsuperabsorbent polymers. The combination of translucency using glass fibers with promoted self-healing prop-erties using superabsorbent polymers was therefore assessed using a direct-mixing technique. The mixturecomposition was optimized, the translucent property was available, multiple cracking was achieved, cracks wereable to visually close and the mechanical properties were regained. This opens up opportunities for furtherapplication of translucent materials, showing self-healing properties.

1. Introduction

Concrete is a material known for its high structural performance, butit has a limited tensile strength, resulting in crack formation during thelifespan of a concrete structure. Furthermore, the presence of cracksendangers the durability as intruding gases and/or fluids will causecorrosion of possible present reinforcements, next to other degradationphenomena. As the concrete structure gradually deteriorates, repairshould be done as quickly as possible. However, the damage may gounnoticed, repairs may be postponed, or in some cases repair is even notpossible due to a lack of accessibility of the structure. Fortunately, con-crete has a passive healing capacity, e.g. autogenous healing. By thecombination of four different healing mechanisms, the cracks in thecementitious material are able to close. The healing mechanisms are (1)the blockage of the cracks by impurities, (2) the swelling of calcium-silicate-hydrates at the crack walls, (3) the further hydration andpozzolanic activity of not yet reacted binder particles, and (4) the cal-cium carbonate crystallization (Edvardsen, 1999; Granger et al., 2007;Snoeck and De Belie, 2019; Snoeck, 2018). Due to a decreasing amount ofunhydrated particles as further hydration occurs in the system with time,the main healing mechanism at later ages will be the calcium carbonatecrystallization (Snoeck and De Belie, 2019; Van Tittelboom et al., 2012).In order to take advantage of this self-healing feature, one needs to

eck).

14 May 2020; Accepted 14 May 2

evier Ltd. This is an open access a

guarantee sufficient building blocks such as the availability of certainhydration products or unhydrated particles. On the other hand, a crackshould be sufficiently narrow in order for healing products to bridge thecrack (Li et al., 2002; Li and Nawy, 2008). Additionally, water needs to beavailable to sustain the healing reactions (Snoeck et al., 2014a; Yang,2008).

In order to limit the crack width, fibers may be added to thecementitious mixture. Multiple cracks with limited crack widths havebeen achieved using synthetic fibers such as polyethylene (PE), poly-propylene (PP), and polyvinyl alcohol (PVA) fibers (Li et al., 2002; Li andNawy, 2008; Snoeck and De Belie, 2015a; Zollo, 1997; Li et al., 1997;Homma et al., 2009). These mixtures were optimized to have narrowcracks up to 30–50 μm (Li and Nawy, 2008; Yang, 2008; Snoeck, 2015).This is a boundary condition for self-healing to efficiently and completelyclose a crack even at later ages in this specific type of strain-hardeningcementitious materials (Li and Nawy, 2008; Yang, 2008; Snoeck,2015). Another possibility is the use of natural fibers, such as flax orhemp, with or without chemical treatment to induce multiple crackingand a sufficient ductility (Snoeck et al., 2015a; Snoeck and De Belie,2012). Both for natural and synthetic fibers, the interaction betweenfiber, cementitious matrix and fiber-matrix interface leads to the wantednarrow crack widths. As the fibers are evenly distributed in the cemen-titious matrix, the position of the cracks will be more evenly spaced in

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rticle under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-

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comparison to traditional reinforcements. This increases the ductility ofthe composite. The bond of the fiber with the matrix is of importance, asit will provide friction, anchorage due to deformation and phys-ical/chemical adhesion during crack formation. The wanted feature is astrain-hardening effect. When a cementitious matrix cracks, the micro-crack will pass several fibers. The tensile stresses are diverted to the fi-bers, bridging the crack. The crack propagation is halted and the tensileforces are relocated. This procedure repeats itself causing multiplemicrocracks to form instead of one big crack. This principle of multiplecracking is the basis for a good autogenous healing capacity upon highstrain deformations and cracking.

On the other hand, as mentioned, water needs to be available totrigger the autogenous healing mechanisms. Water can be provided usingsuperabsorbent polymers (SAPs) (Snoeck et al., 2012a, 2014a; Snoeck,2015; Kim et al., 2010). Able to swell up to hundreds of times their ownweight in aqueous solutions, the SAPs will not only physically seal cracksby their swelling action (Lee et al., 2010, 2016; Snoeck et al., 2012b,2018a), they will stimulate autogenous healing as well when beingincluded in the cementitious mixture (Snoeck, 2015, 2018; Snoeck et al.,2014a). This healing can be sustained for a subsequent healing cycle(Snoeck and De Belie, 2015b) and occurs due to the release of moisture orliquids absorbed by the SAPs. This stored water is released towards thecementitious matrix where it is available for autogenous healing in theform of further hydration and calcium carbonate crystallization.Furthermore, the SAPs also assist in forming a beneficial micro-porositynot only to increase the freeze-thaw resistance (Mechtcherine et al.,2017; Mechtcherine and Reinhardt, 2012; M€onnig et al., 2007), but alsoto increase the ductility due to their crack initiator capacity (Yao et al.,2011). This will cause more multiple cracking with slightly finer cracks.

Next to a self-healing feature, it is interesting to include a translucentcharacteristic in specific cementitious elements. Light always plays animportant role in the daily life. In addition, due to the development ofnew construction processes and the application of new building mate-rials, slender and modern cementitious structures are possible. However,to some, concrete is still a grey and dull material. In response, a newconcept starts to find its way into the concrete society, being the trans-lucency of cementitious materials. How can a cementitious materialbecome more transparent by inducing or conveying light within itscementitious matrix? Glass fibers can be added, to introduce opticalcharacteristics. Moreover, the application of such translucent materialcan be of interest. In current practices, for example, traffic-guiding linesare applied on a hardened concrete road and are sometimes invisible fordrives during harsh weather conditions. A way to include these uponcasting is the application of smart lane separators using light technologyin order to guide the traffic (Saleem et al., 2017). Other utilities such asartificial lighting or data transfer cables are often installed after con-struction works, and can now be included from the start.

One way of including a light-transmitting property is by layering glassfiber mats in the longitudinal direction of the concrete mould, up to atotal volume of 5 volume-percentage (v%). The fiber mats are alternatedwith a fine-grade concrete layer of 2–3 mm when the specimen is cast.Once cured, the element is sawn in blocks perpendicular to the longitu-dinal direction of the fiber mats. In this way, the mats protrude the faceson opposite sides assuring light transmission. The manual placement ofthe mats is labor-intensive and a more efficient way of casting should befound. Another way to produce translucent cementitious materials is byembedding resin elements, consisting of acrylic glass, into the cementi-tious matrix. These resin elements are made separately and directlyplaced into the mould, after which concrete is added. The cost of makingthese elements and carefully placing them, limits wide application inpractice. Furthermore, due to these elements, the load-bearing capacitydecreases and this type of cementitious material can thus only be used ascladding or decorative material (Mainini et al., 2012). Including plasticoptical fibers is another option (Altlomate et al., 2016). In this case, longfibers are manually inserted through the mould, which is labor-intensiveand time-consuming. An idea would be to add glass fibers directly to the

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mix, i.e. the direct mixingmethod. Glass fibers have been investigated foruse in a cementitious material (Snoeck and De Belie, 2015a; Bentur et al.,1985; Larner et al., 1976; Yilmaz and Glasser, 1991), but are not opti-mized to provide multiple cracking behavior and possible self-healingproperties.

Developing a durable self-healing translucent cementitious matrixusing glass fibers could be the first step towards the integration ofdifferent functionalities and applications through one single composite.However, there is the need of an efficient mixing procedure to cope withthe intensive labor and excessive times needed in current molding. Theaim of this research is to investigate the direct-mixing method and thepossible strain-hardening effect using glass fibers to promote autogenoushealing combined with translucency through the glass fibers. An addi-tional improved healing capacity is envisaged by the inclusion of SAPs inthe mixture design.

2. Materials and methods

In this section, the different studied mixtures, types of fibers and SAPsare explained first (2.1), followed by the experiments and investigationon the self-healing properties (2.2). In the next section, the experimentalwork to determine the performance in terms of translucency is described(2.3).

2.1. Studied mixture compositions and materials

The reference mixture was composed out of CEM I 52.5 N (Holcim,Belgium), Class F fly ash (OBBC, Belgium), silica sand M34 with a d50 of170 μm (Sibelco, Belgium), water, polycarboxylate superplasticizer(Glenium 51, 35% concentration, BASF, Belgium), and polyvinyl alcohol(PVA) fibers (2 volume-percent, v%; 1.3 g cm�3; 1.5⋅10�6 kg m�1 ¼ 1.5dtex; 8 mm cutting length; 39 μm filament diameter; 1.2 GPa ¼ 12 cN/dtex tenacity; obtained from Kuraray, Japan). The composition, next toall other studied mixtures are shown in Table 1.

Next to the reference mixture with PVA fibers, mixtures with differentamounts of alkali-resistant (AR) glass fibers (0/1/2/3/4 v%) wereinvestigated. Two different types of AR glass fibers were investigated; amicro type (2.68 g cm�3; 9–12 mm cutting length; filament diameter of14 μm; 1700 MPa tensile strength; obtained from Beton FiberTech,Belgium) and a macro type (same properties but with 36 mm cuttinglength and 19 μm filament diameter leading to a maximum bundlediameter of 540 μm). Mixtures with these glass fibers with and withoutPVA fibers included were investigated. However, one specific consider-ation needs to be taken into account: the possible degradation in analkaline environment of the glass fiber near the interface due to its highsilica content (Ylmaz et al., 1991). Normal glass fibers are susceptible todegradation due to the alkalinity of the cementitious matrix, having a pHvalue of around 13. This degradation may lead to a decrease in overallproperties of both the fiber and the composite. Therefore, the fibers weretreated by the manufacturer to make them alkali-resistant. As a verifi-cation, a degradation study was performed on these AR glass fibers. Thephysical degradation of the surface of the glass fibers was assessed bymeans of microscopic analysis with a stereomicroscope (Leica S8 APO)mounted with a camera (DFC 295). The fibers were first placed in acement filtrate solution and were analyzed after being 56 days, 112 days,168 days and 3 years submerged in a cement filtrate solution. The cementfiltrate solution was prepared using a cement slurry (CEM I 52.5 N) with awater-to-cement ratio of 10 and 24 h of mixing, followed by a subsequentfiltration with particle retention of 12–15 μm. The clear cement filtratewas renewed monthly for the first 6 months. No apparent visual changeor destruction of the surface layer was microscopically seen.

Two SAP types were used; SAP A being a copolymer of acrylamideand sodium acrylate with a particle size of 100� 22 μm, and SAP B beinga cross-linked potassium salt polyacrylate with a particle size of477 � 53 μm (both obtained from BASF, Germany). Both SAPs wereproduced by means of bulk polymerization. The swelling capacity of the

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Table 1The mixture composition of all studied mixtures [kg⋅m�3], showing the amount and type of fiber and/or superabsorbent polymer added in the nomenclature, next to thecement (CEM), fly ash (FA), sand (S), water (W), additional water (Wa) superplasticizer (SPL), fiber (PVA, micro and/or macro), and superabsorbent polymer (SAP)amounts.

CEM FA S W þ Wa SPL PVA micro macro SAP

REF 2 v% PVA 608 608 426 365 5.5 26.0 – – –

1 v% micro 615 615 430 369 5.5 – 26.8 – –

2 v% micro 608 608 426 365 5.5 – 53.6 – –

3 v% micro 602 602 422 361 5.4 – 80.4 – –

4 v% micro 596 596 417 358 5.4 – 107.2 – –

1 v% macro 615 615 430 369 5.5 – – 26.8 –

2 v% macro 608 608 426 365 5.5 – – 53.6 –

3 v% macro 602 602 422 361 5.4 – – 80.4 –

4 v% macro 596 596 417 358 5.4 – – 107.2 –

2 v% PVA þ2 v% macro 596 596 417 358 5.4 26.0 – 53.6 –

2 v% PVA þ3 v% macro 590 590 413 354 5.3 26.0 – 80.4 –

2 v% PVA þ2 v% macro þ0.5 m% SAP A 544 544 381 327 þ 83 4.9 26.0 – 53.6 2.722 v% PVA þ2 v% macro þ0.5 m% SAP B 579 579 406 348 þ 25 5.2 26.0 – 53.6 2.902 v% PVA þ2 v% macro þ1 m% SAP B 563 563 394 338 þ 50 5.1 26.0 – 53.6 5.632 v% PVA þ3 v% macro þ1 m% SAP B 558 558 390 335 þ 49 5.0 26.0 – 80.4 5.58

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SAPs in different solutions can be found in Snoeck (2015) (Snoeck,2015), following the procedures recommended by RILEM (Snoeck et al.,2018b). These SAPs were added on top of a studiedmixture in amounts of0.5 m% (mass-percentage of binder weight) and 1 m%, ideal amounts forpromoting autogenous healing (Snoeck and De Belie, 2019; Snoeck,2018; Snoeck et al., 2014a; Snoeck, 2015). Additional water was addedon top of the mixture to compensate for the loss in workability as theSAPs partly absorb mixing water and store this for internal curing pur-poses (Jensen and Hansen, 2001; Snoeck et al., 2017; Dudziak et al.,2010; Justs et al., 2015). This water is not used prior of final setting andmay not alter the effective water-to-cement ratio (Snoeck et al., 2015b).The absorption capacity in mixing water, as determined by comparingthe workability, amounted to 30.5 g water⋅g�1 SAP A and 8.8 g water⋅g�1

SAP B. This value was verified using microscopic analysis of the macropores, by means of microscopy (Snoeck et al., 2014b) and X-ray tomog-raphy (Snoeck et al., 2016).

The mixing procedure was the following. First, cement, fly ash andSAPs (if included), were dry-mixed for 30 s. Next, water and dissolvedsuperplasticizer were added together and themixing continued for 30 s at140 rpm. The fine silica sand was added in the next 30 s. To ensurehomogeneous dispersion of all components, the mixing speed wasincreased for the following 30 s to 285 rpm. The edges of the mixing bowlwere scraped during 30 s and the mixture was then allowed to rest for60 s. Subsequently, the respective type (or combination) of fiber(s) wasadded while mixing during 30 s at 140 rpm, and the final step was mixingfor 60 s at 285 rpm. Next, the samples (dimensions and amount of rep-etitions in the next sections) were cast in a mould and covered withplastic foil for one day. After demoulding at 24 h, the samples were storedat high relative humidity (95� 5%) and 20� 2 �C till their age of testing.

2.2. Experimental work on self-healing

Specimens with a size of 160 � 40 � 40 mm3 were cast and were cut

Fig. 1. Schematic overview of th

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at an age of 7 days into three 160 � 40 � 10 mm3 samples per specimen.The samples were sawn to expose the glass fibers on the opposite surfacesto induce the translucent effect. The samples were dry-cut to ensure noloss in building blocks for autogenous healing later on and to ensure nochange in microstructural properties due to the use of water which maystimulate hydration and cause a shift in porosity. Next, the specimenswere investigated on their self-healing characteristics. A schematicoverview of the methodology is given in Fig. 1.

The first step was subjecting the specimens with a dimension of 160� 40� 10 mm3 to a four-point-bending test (Walterþ Bai DB 250/15) atan age of 28 days, using a displacement-controlled test at 0.0015 mm s�1

along the vertical loading stage to imitate a quasi-static load condition.The span in between the lower supports measured 140 mm and in be-tween the two loading supports on top 50 mm. The obtained force-vertical-displacement curves were transformed to determine the stress-strain behavior at the bottom of the specimens by means of trigonom-etry, relating the vertical displacement to the strain in the curved lowersurface of the specimens during bending (Snoeck, 2015). In case thespecimens were subjected to healing, the strain was limited to 1% inpreloading. The unloading speed was 5 N s�1. In addition, specimenswere loaded until failure to determine the first-cracking stress and theultimate strain-hardening behavior. The first-cracking stress is defined asthe first occurring drop in stress due to an unstable extension in thematrix fiber tunnel upon microcracking. In addition, the amount ofstrain-hardening being the ductility was investigated. The ductility isdefined as the strain at the bottom of the specimen starting from thestrain related to the first-cracking stress until the strain at ultimate stresswhen strain hardening ends and strain softening starts. For all tests,minimally six samples were studied.

The occurring crack widths were visually monitored using opticalstereo microscopy. The stereomicroscope used was a Leica S8 APOmounted with a DFC 295 camera. Next, the specimens were subjected toa healing condition, being alternative storage in water at 20 � 2 �C for

e healing analysis procedure.

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12 h and in standard laboratory conditions of 60 � 5% RH and 20 � 2 �Cfor the next 12 h. An automated pumping systemwas used to pumpwaterfrom one side to another in 12-h intervals. The water was replaced every7 days. The cracked faces were facing upwards, draining the water out ofthe cracks during dry periods. This side also provides the lowest possi-bility for visual healing of a crack. If the specimens would be put with thecrack facing downwards, more water would be retained in the crack andthe healing products would preferentially form near the crack tip, leadingto a possible overestimation of the visual crack closure.

The healing lasted for a total of 28 days. After the complete healingstage, crack widths were again visually monitored by means of micro-scopic analysis and the specimens preloaded to 1% strain were reloadedin four-point-bending to complete failure to determine the regain in first-cracking stress, as means for calculating the regain in mechanical prop-erties. The regain in first-cracking stress was calculated as the ratio of thefirst-cracking stress upon reloading compared to the first-cracking stressat preloading stage and is expressed as percentage.

2.3. Experimental work on translucency

The translucency was determined on specimens with differentamounts of macro glass fibers added. Two different mixing procedureswere investigated. In this study, the first tested manufacturing procedurewas to include the glass fibers manually and vertically through themould. The second procedure was the direct-mixing method, adding thefibers directly to the mixture, as described above.

In case of the manual insertion method, only one mixture containing 2v% of macro glass fibers was investigated. Adding higher amounts of glassfibers was not feasible due to handling and positioning in the mould.Microglass fibers were not studied due to their short length disabling a propermanual handling. The mould was made from a Styrofoam bottom andfixed wooden spacers providing an inner 160 � 40 mm2 surface and aheight of 10mm. The amount of fibers needed per 160� 40 mm2 face wasdetermined. The fibers were manually, vertically, randomly and evenlyinserted in the Styrofoam bottom, ensuring their fixed vertical position.Next, the reference mixture was poured into the mould and the specimenwas carefully tapped to remove entrapped air. The specimens werecovered with plastic foil. After demoulding at 24 h, the samples withprotruding fiber layout through the material were stored at high relativehumidity (95 � 5%) and 20 � 2 �C till their age of testing. At an age of 7days, the samples were sawn and polished along the bottom and top, toremove the protruding ends of the macro glass fibers and to obtain asmooth surface. Twelve 160 � 40 � 10 mm3 specimens were tested.

In addition, a direct-mixing method was applied by adding the macroglassfibers duringmixing and sawing cured160� 40� 40mm3 samples tothree160�40�10mm3 specimens afterwards. The amount ofmacroglassfibers was varied (0/2/3/4 v%). Per test series, twelve 160� 40� 10mm3

specimens were tested.The amount of translucency was determined by measuring the

amount of light passing through two opposite specimen's surfaces acrossits 10 mm thick dimension. Several pictures were taken using a black-boxprinciple setup. The schematic overview of the setup used in shown inFig. 2. In a frame of plywood, two lamps (40Watt) were positioned. Next,a rubber foam mould was used as specimen holder, enabling a tight fitwith the plywood box. A cardboard black box was put on the specimen toeliminate light pollution from surrounding light sources. The observationof translucency was performed through a small opening in the black box.

Different pictures were made prior and after sample testing at an ageof 28 days and were compared to readings by means of a lux meter(Benetech Digital Lux Meter GM1020) to verify the light intensity havingwavelengths in the range of 400 nm and 700 nm in time throughout thetest campaign. The lux meter was hereby inserted in the small cameraopening and the value did not vary in time, showing that the light in-tensity was constant. The specimens were studied using a camera(Panasonic Lumix DMC-FZ28). The obtained sample pictures were thenstudied bymeans of the software ImageJ. The obtained pictures were first

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desaturated and transformed to grey-level images (0–255). The histo-grams of the grey-level images were transformed into a white-pixel ratio(WPR), taking the sum over the pixels with values in the range of 245 and255, ascribed to the light transmission, over the total amount of pixels inthe range of 0 and 255.

Next to the direct-mixing of the test specimens, a proof-of-conceptdemonstrator was made from a 150 � 150 � 150 mm3 cube containinga mixture with 2 v% of PVA fibers and 3 v% of macro glass fibers usingdirect mixing. The sample was cast, covered with plastic foil, demouldedafter 24 h, and stored at high relative humidity (95� 5%) and 20� 2 �C.At an age of 7 days, the specimens’ height was sawn to 100 mm byremoving layers of 25 mm from the top and the bottom surface. Next, acore of 85 mm was drilled from the center of the specimen, along itsheight. In a next step, the remaining surfaces were also sawn to remove a25 mm layer. In the end, a hollow 100 � 100 � 100 mm3 cube wasobtained, in which the hollow core allowed to insert a light bulb of 40Watt.

3. Results and discussion

In the first part, the mechanical characteristics and regain in me-chanical properties for all studied mixtures are discussed (3.1), followedby the visual monitoring of the self-healing properties (3.2) and trans-lucent properties (3.3).

3.1. Mechanical properties and regain in mechanical properties due to self-healing

One of the three criteria to have efficient autogenous healing is thelimitation in crack width. Multiple microcracks are the result of thestrain-hardening behavior of the fiber-reinforced cementitious compos-ite, as analyzed by the mechanical behavior after performing four-point-bending tests. The stress-strain relation of specimens containing microglass fibers, macro glass fibers and a combination of macro glass fibersand PVA fibers were compared to reference samples containing 2 v% PVAfibers, fully characterized in terms of mechanical behavior and self-healing (Snoeck and De Belie, 2019; Li et al., 2002; Li and Nawy,2008; Snoeck, 2015; Yang et al., 2009). SAPs were added to mixturescontaining macro glass fibers and PVA fibers. The mechanical propertiesfor all studied mixtures are given in Table 2.

The reference mixture containing 2 v% PVA fibers showed analogousresults as found in literature. Results in literature show mechanicalcharacteristics of mixtures with only PVA fibers of 4.8 � 0.6 MPa to5.9 � 0.6% for the first-cracking-stress, 2.4 � 0.1% to 3.8 � 0.6% forductility strain, and a regain in first-cracking-stress of 40 � 8% to45� 7% (Yang, 2008; Snoeck, 2015). In literature, typical strains are 1%and 4% if 1.2 v% and 2 v% of PVA fibers, with an analogous mixturedesign, were added (Li et al., 2002). The regain in first-cracking stress inthis research amounted to 44 � 3%. Stored in standard laboratory con-ditions, no healing would occur in SAP-less samples. This is due to theunavailability of liquid water, needed in the self-healing mechanisms.

Different mixtures containing 1, 2, 3 and 4 v% of micro glass fiberswere investigated. None of those specimens showed strain hardening.Instant strain softening was observed related to a brittle failure of thefibers in each specimen, due to the strong bond with the cementitiousmatrix. A higher first-cracking stress is found inmixtures withmicro glassfibers compared to mixtures with PVA fibers only due to the higher bondwith the matrix of the micro glass fibers compared to the PVA fibers,leading to a stronger overall composite. The higher forces are also due tothe higher modulus of elasticity of glass fibers compared to PVA fibers. Asno ductile behavior was noticed, no study on the healing capacity wasperformed.

Including macro glass fibers in the mixture leads to a strain-hardeningeffect. However, a noteworthy variance was found in the test results dueto the relative large fiber dimensions compared to the specimen di-mensions. The macro glass fibers have a total length of 36 mm, making it

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Fig. 2. (a) Schematic overview of the used setup to verify the translucency with (1) the plywood frame, (2) lamps, (3) specimen holder, and (4) black-box transfer, and(b) the top view with camera opening.

D. Snoeck et al. Developments in the Built Environment 3 (2020) 100012

hard to disperse them properly in a cross section of 40 mm by 40 mm.Debonding of the macro bundle was the main cause of failure. In the end,2 to 7 cracks were observed, with varying crack widths of around100 μm–1200 μm, which is too wide for proper autogenous healing tooccur. Therefore, as the healing would be minimal, the specimens werenot studied for their healing capacity. There is an optimum of 2 v% to 3 v% of macro glass fibers in terms of good ductile behavior. A too highamount results in a decrease in strength. It was therefore opted to study 2v% and 3 v% in the subsequent sample series in which the macro glassfibers were combined with PVA fibers.

Strain hardening was only possible using the macro glass fibers.However, the amount of strain hardening needed to guarantee the self-healing behavior needed to be improved by combining respectively 2and 3 v% of glass fibers with 2 v% PVA fibers. In PVA fiber samples, therewas a high scatter in ductility results. There was no ductility observed insamples with micro glass fibers, a slight ductility in specimens withmacro glass fibers and good ductility in the combination of PVA fibersandmacro glass fibers. No significant differences are foundwhen sampleswith PVA fibers only and the combination of PVA fibers and 2 v% ofmacro glass fibers are compared, in terms of mechanical properties. Anincrease in first-cracking stress is observed upon adding 3 v% of macro

Table 2The first-cracking stress σfc [MPa], ductility as a measurfirst-cracking stress SH [%], for all studied mixtures. Foamount and type of fiber, and the possible addition of S

n/a: not investigated as there was no observed strain ductcracks (macro glass fibers)were formed

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glass fibers. This is due to the in-total larger amount of fibers, leading to astronger overall composite. More crack clusters were observed in thespecimen containing 3 v% of macro glass fibers. The cracks in the latterspecimen were concentrated over a shorter distance compared to thespecimen with 2 v% of macro glass fibers. The long macro fiber is activeover multiple cracks and abundant multiple cracking was observed,comparable to the reference sample containing 2 v% of PVA fibers only.

Due to saw cutting the specimens, some fibers will show a shorterlength. Furthermore, fibers perpendicular to the saw-cut will not effec-tively contribute to the strain-hardening capacity. Due to the inclusion oflarger fibers compared to the PVA fibers, some clustering may haveoccurred. This was visually seen on the surfaces of the specimens, espe-cially when adding high amounts of macro glass fibers.

SAPs decrease the overall mechanical strength due to their macro-pore formation but the differences are not significant. The inclusion ofSAPs improves the ductility (up to 4.10 � 0.91%) due to their crackinitiator capability (Yao et al., 2011). As mentioned, when too highamounts of SAPs are added, the strength may be impaired (Snoeck et al.,2014b; Hasholt et al., 2012). Different amounts of SAPs were added,being 0.5 m% SAP A, 0.5 m% SAP B and 1 m% SAP B, respectively,expressed as mass percentage of binder weight, as these amounts are

e for multiple cracking strain MC [%] and regain inr all mixture compositions, the variables being theAPs, are given.

ility (micro glass fibers) and/or too wide unhealable

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D. Snoeck et al. Developments in the Built Environment 3 (2020) 100012

sufficient to promote autogenous healing (Snoeck and De Belie, 2019).When including 1 m% of SAP B, the observed ductility was increasedmost compared to the SAP-less specimen.

As mentioned, two different approaches for measuring the healingcapacity were conducted, by checking the regain in mechanical proper-ties and by monitoring the visual closure of the cracks. The latter will bediscussed in the next section. Autogenous healing was found in allspecimens, with and without SAPs. The specimens containing SAPs,however, did show an improved healing capacity and regain in me-chanical properties. The regain in first-cracking stress of SAP-less samples(44 � 3%) improved up to (60 � 5%) in samples with 1 m% of SAP B.This is due to a stimulated further hydration in 1 m% SAP B samples,amounting to 39% more hydration compared to SAP-less specimens(Snoeck et al., 2020). As there is less stimulated further hydration insamples with 0.5 m% of SAP A (25% more hydration as determined onanalogous specimens but in prior research (Snoeck et al., 2020)) and0.5 m% of SAP B (19% more hydration in prior research (Snoeck et al.,2020)) compared to a mixture with 1 m% SAP B (39% more hydrationdetermined in prior research (Snoeck et al., 2020)), the regain in me-chanical properties (52 � 3% and 53 � 4%, respectively) were slightlylower than upon addition of 1 m% of SAP B (60 � 5%) but still highercompared to the SAP-less reference (44 � 3%).

In literature, mixtures with PVA fibers and SAPs have shown a first-cracking-stress of 4.9 � 1.5 MPa, 5.1 � 1.4 MPa, and 4.9 � 0.9 MPa forsamples with 0.5m%SAPA, 0.5m%SAP B, and 1m%SAP B, respectively(Snoeck, 2015). The ductility in thosemixtures is 3.5� 0.4%, 3.5� 0.3%,and 3.8 � 0.4%, respectively (Snoeck, 2015). The found values in thisresearch correspond to these values found for specimens studied in earlierresearch. The regain inmechanical properties found in literature amountsto 65� 2MPa, 69� 3MPa, and 86� 8% for samples with 0.5 m% SAP A,0.5 m% SAP B, and 1 m% SAP B, respectively (Snoeck et al., 2014a;Snoeck, 2015). The values for the regain inmechanical properties found inthis research are slightly lower, possibly due to the inclusion of the macroglass fibers, limiting the formation of healing products due to the smoothsurface of the macro glass fibers. However, the healing capacity is stillhigher compared to the reference.

3.2. Visual closure due to self-healing observed by microscopic analysis

The visual crack width closure is shown in Fig. 3. On this graph, the

Fig. 3. (a) Visual final crack width [μm] after healing compared to the initial crack wmixtures. For means of comparison, dashed trend lines are added.

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initial crack widths before healing were compared to the remaining crackwidths after 28 days of healing. These results are depicted compared to abisector showing no healing (left-hand side in Fig. 3a) and as the per-centage of visual closure shown for comparative reasons (right-hand sidein Fig. 3b). All samples studied had 2 v% of PVA fibers, 2 v% of macroglass fibers and a varying amount of SAP A or SAP B (0/0.5 m% SAP A or0/0.5/1 m% SAP B).

As could be expected, smaller cracks have a higher probability to becompletely closed due to autogenous healing, in all specimens studied. Inreference samples, most cracks up to 30 μm closed completely. In SAPspecimens, this healing is sustained to more than 50 μm. For larger crackwidths, the healing is becoming nonexistent in reference samples from100 μm onwards. For SAP samples with low amounts up to 0.5 m% ofSAP, this amount of visual crack closure is slightly higher. Whenincluding 1 m% of SAP B, this healing is further and beneficially pro-moted and more healing is visually seen, mostly in the form of calciumcarbonate crystallization. If 1 m% of SAP A would be added, the overallstrength of the material would decrease too much due to a pronouncedadditional formation of macro pores due to their high mixing water up-take compared to SAP B (Snoeck et al., 2014a, 2014b). The same holdstrue for mixtures with even higher amounts of SAP B. Those mixtureswere therefore not studied.

Compared to the reference sample, the average crack closure wasmore noteworthy in SAP specimens. Additionally, due to the crackinitiator capability of the SAPs, smaller crack widths are generally foundin SAP samples, leading to a better regain in mechanical properties assmaller cracks are healed better by inclusion of SAPs. SAP B seems toperform better compared to SAP A in terms of stimulated autogenoushealing capacity. The average crack width in the SAP-less samples loadedto complete failure was 62 μm, while for adding 0.5 m% SAP A or SAP Band 1 m% SAP B this average was 46, 47 and 42 μm, respectively.

Some calcium carbonate crystals were observed at the circumferenceof the exposed glass fibers, but most in the presence of PVA fibers. Due tothe smooth fiber surface of the macro glass fibers, the cracks convertedand diverted slightly. The same behavior of acting as a nucleation site forhealing products is seen in samples with PVA fibers only (Snoeck et al.,2014a). Overall, the same trend is seen in literature, where SAPs are alsoable to promote visual closure of the cracks (Snoeck and De Belie, 2019;Snoeck et al., 2014a; Snoeck, 2015; Snoeck and De Belie, 2015b; Snoecket al., 2016). The glass fibers seem not to influence these results.

idth [μm] and (b) percentage of visual closure of the initial cracks, for all studied

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Fig. 4. (a) Visual translucency with an external light source, and (b) with an internal light source, showing the protruding glass fibers transferring the light from insideto outside.

D. Snoeck et al. Developments in the Built Environment 3 (2020) 100012

3.3. Translucent effect and proof-of-concept

As mentioned in the introduction, glass fibers have the capacity totransmit light through their inner core and different manufacturingprocedures exist. In this study, the first manufacturing procedure was toinclude the glass fibers manually and vertically through the mould,causing a protruding layout of the fibers. This method guarantees themaximal translucent effect. This labor-intensive method is currently usedin practice to have optimal translucent properties from the two oppositefaces, meaning along the fiber axis. As an addition, a direct-mixingmethod was applied by adding the fibers during mixing and exposingthem by sawing the cured samples afterwards. Both methods werecompared. The sawing action is an additional manual labor but does notoutweigh the manual insertion labor. Only fibers going through bothopposite faces of the specimen were transferring light. This means thatnot all fibers were active for transmitting light. In addition, the visualappearances were more random, as can be seen in the proof-of-concept inFig. 4. The translucent properties are shown when there is external light(Fig. 4a), and internal light (one internal light bulb of 40Watt in Fig. 4b).In case of external light, some macro glass fibers can be seen at theexterior surface of the hollow cube, and these will not transfer the light asefficiently as the protruding macro glass fibers, clearly visible with aninternal light source.

In order to quantify the translucency effect, the WPR was calculatedfrom analyzing the histogram of the black-box images obtained fromtwelve 160 � 40 � 10 mm3 samples. Studying samples without macroglass fibers resulted in a WPR of zero, meaning that no light could berecorded. Furthermore, there was a logical correlation between theamount of macro glass fibers added and the total visual transmittance oflight. When the fibers were manually inserted in the mould, the WPR was5.38 � 0.42% (n ¼ 12 measurements) when using 2 v% of macro glassfibers. Using the direct-mixing method, lower values were obtained. TheWPR varied from 1.33 � 0.92% (n ¼ 12 measurements) over3.90 � 0.85% (n ¼ 12) to 4.71 � 1.09% (n ¼ 12) for samples with 2, 3and 4 v% of macro glass fibers added, respectively. Note the large vari-ability due to the variable direct-mixing method. Only fibers perpen-dicular to the specimen's longitudinal axis increased the white-pixel ratio(WPR) significantly. This can be overcome by looking into different waysof pouring the fibers, guaranteeing the flow in one specific direction uponcasting. This is subject for further research. There was no direct effectnoticed in translucency prior and after healing. The only effect was aslight reflection of light on the white calcium carbonate crystals, but the

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WPR did not vary significantly. The translucent effect is limited, relatedto the thickness of the sample and the length of the fiber used.

4. Conclusions

Combining two different properties, being self-healing and trans-lucency, was achieved by using glass fibers in a strain-hardening cemen-titious composite. A ductile strain-hardening behavior was observedwhich promoted autogenous healing. Based on the results obtained bystudying both characteristics, following conclusions can be drawn:

- The direct-mixing method leads to a translucent effect and is lesslabor-intensive compared to manual insertion of the glass fibers.

- Strain hardening was only feasible when using macro glass fibers, andnot when applying micro glass fibers. Further interface tailoringwould be necessary to improve the corresponding multiple crackingand the strain-hardening capacity.

- Adding an amount of 2 v% PVA fibers to mixtures containing macroglassfibers increases the overall strain-hardening capacity extensively.

- Autogenous healing and improved autogenous healing by addingSAPs combined with translucency via the glass fibers has beenobserved. The exposed PVA fibers tend to promote nucleation ofcalcium carbonate crystals, stitching the crack. The macro glass fibersare too smooth and have a different composition compared to the PVAfibers, and they do not promote this nucleation behavior.

- SAPs act as crack initiator, increasing the ductile behavior. This leadsto the formation of more narrow cracks, easier to be healed with theself-healing mechanisms.

- The translucent effect in the cementitious material is proportional tothe volume percentage of macro glass fibers added when using thedirect-mixing method. A maximum of 3 v% of macro glass fiberscombined with 2 v% PVA fibers was achievable and led to goodproperties in terms of visual healing and a translucent effect of4.71 � 1.09%.

- Adding 1 m% of SAP B to the mixture leads to a regain in mechanicalproperties up to 60 � 5%, compared to 44 � 3% for a SAP-lessspecimen.

- Creating a cementitious mixture with self-healing and translucentproperties is a first step towards the development of newmaterials forseveral applications where translucent properties are useful.

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Data availability statement

The datasets generated during and/or analyzed during the currentstudy are available from the corresponding author on reasonable request.

Declaration of competing interest

The authors declare that they have no known competing financialinterests or personal relationships that could have appeared to influencethe work reported in this paper.

Acknowledgements

As a Postdoctoral Research Fellow of the Research Foundation-Flan-ders (FWO-Vlaanderen), D. Snoeckwould like to thank the foundation forthe financial support (12J3620N). We wish to thank Beton FiberTech,Belgium, for providing the glass fibers. We also want to thank BASF,Germany, for providing the SAPs.

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