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# Automated in-situ metrology of the areal morphogenetic transition of cement mortar at early ages

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Łukasz Sadowski<sup>a,*</sup>, Thomas G. Mathia<sup>b</sup>

## ARTICLE INFO

**Article history:**

Received 29 July 2019

Received in revised form 30 October 2019

Accepted 1 November 2019

Available online 9 November 2019

**Keywords:**

Automation

Metrology

Cement mortar

Surface morphogenesis

Early ages

Morphology

## ABSTRACT

This study focuses on the automated in-situ metrology of the superficial morphological evolution of the surface of cement mortar at early ages. This was carried out at different stages of the complex dynamic mechanism process of solidification. Automated portable non-contact 3D Light Amplification using the Stimulated Emission of Radiation (LASER) scanning technique was applied in order to determine the superficial morphological transitional phases during early age surface morphogenesis. The most pertinent discoveries were determined using two transitions and three transitional phases. These discoveries were visualized in the form of isometric images of vertical altitude transitions and also in the form of directionality in the morphogenesis of lateral transitions. A proposal of the dynamic mechanism was presented for better process control that explores the modelling and implementation of self-architecting systems of mortar at early ages.

© 2019 The Author(s). Published by Elsevier Ltd. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).

## 1. Introduction

Fresh mortar can generally be defined as a mixture of ordinary Portland cement, sand and water. It forms a heterogeneous material. Proper handling of the surface of mortar at early ages is important. This formation affects the superficial morphological, rheological and physicochemical states. This is a complicated three phasic system. In this system, wettability between the cement, sand and water is crucial [1]. The thermo-mechanical assessment of cement mortar determines its functional properties [2]. It also determines the suitability of the surface of the mortar in relation to the concerned medium and required future performance [3–5]. The behavior of fresh mortar during the filling of formwork, compaction and leveling has to be controlled. It is necessary to provide the required durability, stability or adequate visual characteristics of the final hardened material. It is still very difficult to characterize the morphogenesis of the surface of cement mortar at early ages [6,7]. Most of the latest research is mainly related to phenomena such as shrinkage [8,9], cracking [10], thermal deformations [11], stiffness [12], fracturing [13], setting [14], self-healing properties [15], compressive strength [16], elastic modulus [17], or hydration [18] and its kinetics [19]. From the

available test methods, ultrasonics [20,21], highly nonlinear solitary waves [22–24], shear wave reflection [25], guided surface waves [26], embedded piezoelectric transducers [27], isothermal calorimetry [28], or permeability and crack closing tests [29] have recently been used the most. In-situ metrological systems are being more frequently used by researchers to characterize the surface of cementitious materials in various applications [30–31]. From a morphological point of view, automated in-situ non-contact dimensional multi-scale metrology should be applied [32–36].

Fig. 1 presents smartphone raw pictures of visual modifications in the morphology of cement mortar. These changes are easily visible. Significant changes on the surface of the cement mortar start immediately after casting and can be optically visible (Fig. 1). The dynamics of the emerging and decreasing hills of depicting aggregates and the spreading and retraction of “lakes”, emphasized by blue arrows, can be seen. Similar to the evolution of the surface of concrete, described in detail in [37], the surface of the cement mortar initially looks like a viscous suspension, but 1800 s later it becomes a solid material.

Thus, the study is dedicated to the automatic revealing and measuring of any evident superficial morphological evolution and to also discriminate its transitional phases during the solidification process of the surface of cement mortar at early ages. According to the authors, knowledge of the areal morphogenetic transitions of cement mortar at early ages have not yet been

<footnote><sup>a</sup>Faculty of Civil Engineering, Wrocław University of Science and Technology, Wybrzeże Wyspiańskiego 27, 50-370 Wrocław, Poland</footnote>

<footnote><sup>b</sup>Laboratoire de Tribologie et Dynamique des Systèmes, École Centrale de Lyon, 69134 Écully, France</footnote>

<footnote>* Corresponding author.</footnote>

<footnote>E-mail addresses: Łukasz.Sadowski@pwr.edu.pl (Ł. Sadowski), Thomas. Mathia@ec-lyon.fr (T.G. Mathia).</footnote>
<figure><img src="image_3.png" /><figcaption>**Fig. 1.** Smartphone raw pictures of visual modifications in the morphology of cement mortar showing the dynamics of the emerging and decreasing hills (emphasized by red arrows, end with “●”) of depicting aggregates and also the spreading and retraction of lakes (emphasized by blue arrows that end with “♦”). Only the lateral scale is seen. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)</figcaption></figure>

measured, quantified or investigated in detail. The morphologies were analyzed at different in-between stages. This research also validates the suitability of portable non-contact 3D Light Amplification by the Stimulated Emission of Radiation (LASER) scanner for this purpose [33,37,38]. The most significant results, in the form of isometric visualizations of vertical altitude transitions and directionality in the morphogenesis of lateral transitions, are discussed. Consequently, there can be seen to be research gap regarding automated in-situ metrology using an Unmanned Ground Morphoscanning Vehicle (UGMV) [39].

## 2. Materials and methods

Ordinary cement mortar was selected for the experiment. The ingredients used to prepare the investigated mortar were as follows:

* 276 kg/m³ of type CEM I 42.5 R Portland cement (Cement Ożarów S.A., CRH plc group Ożarów, Poland) with a bulk density of 1 106 kg/m³ and surface area of 416 m²/kg (this complies with EN197-1:2011 [40]),

* 1599 kg/m³ of dried quartz sand (mineral mine "MARGO", Mietków, Poland) with a bulk density of 1 497 kg/m³ containing grains with a maximum diameter of 2 mm,

* 138 kg/m³ of tap water.

The water-cement ratio was equal to 0.5 (mass ratio). The consistency of the fresh mortar was measured using the flow table test according to EN 1015-3 [41]. The obtained consistency of the mortar was liquid (a flow diameter equal to 15 cm). Thus, the expected changes of surface morphology can be well seen. As the batch water, tap water was used. The granular analysis (sieve method) of sand is presented in Fig. 2.

A mixing procedure based on EN 480-1 [42] was adopted. The mixer was first wiped inside with a damp cloth. Then, the dry components (sand and cement) were introduced to the mixer. The mixing was finished after 2 min (until they were homogenous). After that, the water was slowly added to the mix. The mixing of the mortar took about 3 min. The prepared mixture was then poured into a 150x150x40 mm oiled mould. In order to see the changes on the surface, the mix was not specially vibrated. Moreover, the surface of the cement mortar was not specially treated. It was patch grabbed and left after casting to obtain an appropriate flat surface for the automated in-situ metrological investigation. This is the most commonly used surface treatment method (due to economic reasons). As pointed out in [43], one of the most fundamental questions in contact mechanics is the knowledge of the size distribution of contact spots.

A specially designed measuring device in the form of an automated non-contact 3D LASER scanner was used for the

measurements (Fig. 3). Due to the fact that in previous research the surface morphology stabilizes after 1800 s [37], the current sample was scanned after 3600 s from the start and then at time intervals of 120 s. It should be highlighted that the scanning time of 3600 s will be mostly within the period of initial reaction of cement hydration, which as reported by Bullard et al. [44] takes approximately one hour. After that, a period of slow reaction starts and takes another one hour. A part of the investigated surface with a size of 50 × 50 mm was selected for further analysis in order to avoid the boundary effect. In total, 30 surface morphologies were measured. A similar scanning procedure has recently been more frequently applied in concrete surface metrology, e.g. in topography studies of concrete wear by ice [45], for the direct measurement of the surface area properties of regular and irregular aggregates used in typical asphalt mixtures [46], or for the assessment of the surface texture of pavements [47,48]. The ambient air temperature during the investigations was +20 °C (±1°C) and the air relative humidity was equal to 60% (±5%). These conditions were distinguished at around 1 m over the investigated surface.

In the implemented Unmanned Ground Morphoscanning Vehicle (UGMV) automated in-situ metrological system (Fig. 3c), an Industrial Vision Camera (IVC) was used. The maximum performance of the IVC camera was equal to 5000 profiles/s. A red diode LASER (wavelength λ = 658 nm) was also used. A microcontroller for image segmentation was applied and the triangulation angle (σ) was equal to 53°. The lateral and vertical resolution was equal to 0.01 mm. The uncertainty did not exceed 0.01 mm. The calibration was performed using the calibration matrix and a south-shape target was used for this purpose. Longitudinal scanning was carried out automatically using a linear guide. The linear guide was joined with an encoder and was used for this purpose. As pointed out in [49], the limitations of the lenses, such as distortions, aberrations, as well as the Modulation Transfer Function (MTF) and its vertical resolution, were taken into account. The morphology of the surface of the cement mortar within an area of 50 × 50 mm was measured. Using the above mentioned test settings, the single measurement took less than 60 s. The results of each measurement were obtained in the form of a cloud of points. After finishing the measurements, the test results were sent to a computer, saved in "*.csv" and converted to "*.sur" format. Before further processing, the data was levelled. As pointed out in [50,51], the surface morphology of cementitious materials can only be considered with primary parameters. Thus, data filtering was avoided in this analysis. Finally, the data was analyzed in MountainsMap® Premium 7.2 Digital Surf software [52] according to ISO 25178 [53].

## 3. Results and discussion

For scientific and technological reasons, the most noteworthy surfaces of the cement mortar were carefully selected and then
<figure><img src="image_4.png" /><figcaption>Fig. 2. Granular analysis (sieve method) of: a) cement type CEM I 42.5 R cement, b) water washed river sand.</figcaption></figure>

<figure><img src="image_5.png" /><figcaption>Fig. 3. View of: a) scheme of the 3D LASER scanning technique [38], b) optical view of the fragment of the analyzed surface, c) Unmanned Ground Morphoscanning Vehicle (UGMV) used for automated in-situ metrology.</figcaption></figure>

analyzed following a recognized procedure. For engineering reasons, the isometric visualizations of vertical altitude transitions (cf. infra 3.1) and the directionality in the morphogenesis of lateral transitions (cf. infra 3.2) were collected and analyzed.

### 3.1. Isometric visualizations of vertical altitude transitions

Fig. 4 presents significant archetypal isometric visualizations of the vertical altitude transitions of the cement mortar surface. It is
visible from this figure that significant changes on the surface of the mortar start at the time of 720 s after mixing. From a metrological perspective, the surface of the cement mortar is initially relatively viscous. After 1440 s, it changed to a more condensed

phase. These variations are quicker than for the surface of Light-weight Concrete (LWC), which according to [37], usually takes around 30 min. The model description will be described later in the article.

<figure><img src="image_6.png" /><figcaption>**Fig. 4.** 3D island pertinent visualizations versus the time of the cement mortar transitional surface morphology stages showing morphogenesis at early ages (during first 1 h).</figcaption></figure>

<figure><img src="image_7.png" /><figcaption>**Fig. 5.** Kinetics of the visualizations of the 3D islands of the cement mortar transitional stages in surface morphology kinetics at early ages of mortar surface morphogenesis (threshold 1.60 mm over the lowest point of the surface) showing three fundamental phases.</figcaption></figure>

<figure><img src="image_8.png" /><figcaption>**Fig. 6.** The adopted procedure of evaluating the texture-aspect ratio of the surface morphology (Str): a) autocorrelation function of the surface, b) threshold autocorrelation at 0.2 (the black spots are above the threshold), c) threshold boundary of the central threshold portion, d) polar coordinates leading to the autocorrelation lengths in different directions (based on ISO 25178 [53]).</figcaption></figure>
Based on the analysis presented in Figs. 4 and 5, it can be observed that the early age superficial morphological evolution process of mortar surface isotropy may be divided into two transitions and three transitional phases. Phase 1 starts immediately after mixing and takes until $t = 600$ s. At the transition between phase 1 and 2, the maximum height of the islands increases from 0.1 mm to 0.5 mm. The second transition is visible at the time of 2400 s. At the transition between phases 2 and 3, the maximum height of the islands, as is the case with the first transition, increases from 0.1 mm to 0.5 mm. There is a need to study this directionality phenomena in the morphogenesis of lateral transitions.

## 3.2. Directionality in the morphogenesis of lateral transitions

The lateral or horizontal coincidence of transitional evolutions during the early stages of solidification with regards to morphologically oriented surface changes are also depicted. The degree of isotropy was measured and evaluated according to ISO 25178 [53]. The adopted procedure of evaluating the texture-aspect ratio of the surface morphology (Str) is presented in Fig. 6. The fundamental algorithm is based on the form of the surface elimination. The autocorrelation function of surfaces ACF ($t_x$, $t_y$) is then calculated. Binary thresholding of the ACF ($t_x$, $t_y$), with a default threshold at 0.2, is also executed (based on ISO 25178 [53]).

<figure><img src="image_9.png" /><figcaption>Fig. 7. Kinetics of directionality in the morphogenesis of cement mortar surface isotropy changes at early ages illustrated with a polar diagram during morphogenesis showing lateral transitions in three transitional phases.</figcaption></figure>
<figure><img src="image_10.png" /><figcaption>Fig. 8. Proposal of a dynamic mechanism of morphogenetic transition due to surface rheology, internal stresses, mixing, water exudation film formation, physical chemistry and the roughness of concerned surfaces (scales are not respected but proportions are).</figcaption></figure>

According to Fig. 6, as a ratio of the minor ellipse axis length ($R_{min}$), the major ellipse axis length ($R_{max}$) and the texture-aspect ratio of the surface morphology (Str) can be evaluated [53]:

$$Str = \frac{R_{min}}{R_{max}} \qquad (1)$$

The morphology of isotropic surfaces is characterized by Str values closer to 1. Anisotropic topography, which is perfectly monodirectionally oriented, obtains Str values close to 0. A perfect isotropic surface of cement mortar probably does not exist. In the case of cement mortar, which is a heterogeneous mix, from a mathematical morphology point of view, it refers to the surface with an identical topography, regardless of the analyzed direction. The observed kinetics of directionality in the morphogenesis of cement mortar surface isotropy changes at early ages are presented in Fig. 7.

The analysis presented in Fig. 5 confirms that the superficial morphological evolution process of mortar surface isotropy can be divided into three phases (cf. supra Fig. 4). During Phase 1, morphological isotropy increases from Str = 0.24 to Str = 0.26. At this high morphological mobility phase, cement and sand particles are separated by water and probably offer low friction from full-film lubrication to the boundary regime [54,55]. In the second phase (Phase 2), which took place between 720 and 2400 s, the surface morphology is still moving. After approximately 2400 s from the start of the measurements (at which the Str = 0.28), a stable period of slow reaction of hydration begins and the superficial morphology of the surface of the cement mortar is calming down (Phase 3).

### 3.3. Proposal of a dynamic mechanism of morphogenetic transition

Based on the performed automated in-situ metrological investigations in Fig. 8, the proposal of a dynamic mechanism of morphogenetic transition due to surface rheology is presented.

The first phase starts immediately after mixing and takes until t = 600 s. Coupling of liquid flow exudation from the mortar cement mixture and the surface behavior of gravel occurs by means of the tangential stress boundary condition during densification of the cement and sand. This mechanism probably operates at the first transition. The movement of the surface morphology within the first two phases and also the presence of the first transition may be associated with the first stage of the hydration process (initial reaction). The second transition is visible at the time of 2400 s. The second morphological transition is probably due to the progression of the gravitation flow and also the expulsion of heaps and gravels that is accompanied by the second increase of the altitudes of islands. This time (2400 s) is a little bit faster than the usual start of the period of slow reaction of cement hydration, which as reported by Bullard et al. [44] starts approximately one hour after casting the specimen. The transition from the initial reaction to the slow reaction measured on the surface of the cement mortar seems to appear faster than the transition

measured inside the specimen by isothermal calorimetry. However, according to Bullard et al. [44], the beginning and ending of the hydration stages are still difficult to identify precisely. This highlights the fact that in future studies the morphogenesis cannot be evaluated, apart from the reactions that occur during hardening. However, it has to be pointed out that the focus in this article was placed on morphology changes and that the chemical behavior of the surface of cement mortar was not treated. In the future it is advisable to investigate the effect of different admixtures on the areal morphogenetic transition of cement mortar at early ages. Based on the analysis of the results presented by Fernández et al. [56], Cultrone et al. [57] and Cizer et al. [58], it is especially advisable to evaluate the behavior of mortars modified with nanoparticles (e.g. nanosilica), lime, pozzolana, air-entraining additives, or different types of superplasticizers (e.g. based on polycarboxylate ether).

### 4. Conclusions

It was metrologically demonstrated that the superficial morphological evolution of cement mortar during the manufacturing process is made possible using automated in-situ metrology. In the modern version of the Unmanned Ground Morphoscanning Vehicle (UGMV) mentioned above, a 3D LASER was implemented. Following superficial morphological evolution, three different transitional stages were identified at the early age formation of the surface of the cement mortar. Horizontal morphological evolution was analyzed by means of the texture-aspect ratio of the surface morphology (Str). The most important results from the point of view of surface morphology are:

* Coupling of liquid flow exudation from the mortar cement mixture and the surface behavior of gravel occurs by means of the tangential stress boundary condition during densification of cement and sand. This mechanism probably operates at the first transition. The observed transitions are irreversible in a three phasic mixture,

* The proposal of a model of a dynamic mechanism of morphogenetic transition with regards to surface rheology, internal stresses, mixing, water exudation film formation, physical chemistry and the roughness of concerned surfaces. This hypothetical model has to be developed and optimized,

* The monitoring of solidification for the predictive modeling of surface morphology, or the self-tuning adaptive control of the process should be explored further.

### Declaration of Competing Interest

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.
Acknowledgements

The authors would like to thank Prof. Jacek Reiner for building a 3D LASER scanner and also Mr. Zbigniew Żelazny, Mr. Mateusz Kupczyk, Mr. Sławomir Czarnecki, Prof. Jerzy Hola and Prof. Piotr Wrzecioniarz for their participation in the constructing of the Unmanned Ground Morphoscanning Vehicle (UGMV), as well as Mr. François Blateyron for his support in using MountainsMap® Premium 7.2.

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