Disertation-Final Version2

DISSERTATION THESIS
THE INFLUENCE OF FINE PARTICLES IN

RHEOLOGICAL BEHAVIOR OF FRESH
MORTAR PASTE
Scientific coordinators: Postgraduate student:

Prof. dr. ing. Belén González Fonteboa Ing. Nemeș Cristina-Raluca
Prof. dr. ing. Diego Carro López
Prof. dr. ing. Julietta Domșa
THE INFLUENCE OF FINE PARTICLES IN THE
RHEOLOGICAL BEHAVIOUR OF MORTAR
PASTE
Nemes Cristina-Raluca
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Abstract
This paper focuses on studying the incorporation of fine particles less than 0.125 mm in the
manufacture of self-compacting mortar paste using natural and recycled fine particles. The mixtures
were adjusted with w/c ratio of 0,4 and a superplasticizer dosage of 0,12, and each natural and
recycled fine matter was added in a ratio of 20, 30, 40 and 45% of the total volume. The rheological
tests, stress grow test and flow curve test, were carried out on fresh state at 32’ and 52’ from the
first contact. There were used three types of fines: first type without being subjected to a mix
before, the second type was subjected to 5’ mix and the third type was subjected to 15’ mix before
usage. After generating the test, I processed the data and come to the following conclusions: the
Modified-Bingham model provides well-defined representation for mortar paste; the values of yield
stress increased with the incorporation of a higher solid volume fraction of FNA and FRA; after a
longer mixing time in preparation of SCC, the aggregates will generate more fines particle which
can jeopardizes the loss of SCC characteristics. Up to 30% the FRA does not influence the
rheological behavior of paste with less mixing time than 15 minutes.
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Resume
Lucrarea de față abordează studierea influenței particulelor fine mai mici de 0,125 mm în
comportamentul reologic al pastei de mortar autocompactant folosind agregate naturale și reciclate.
Alegerea acestei teme a fost motivată de un fenomen relativ nou, respectiv posibilitatea utilizării
agregatelor reciclate, provenite din demolări, în alcătuirea betonului autocompactant, lucrarea
propunându-și să studieze în ce măsură influențează generarea particulelor fine, în timpul
amestecului, lucrabilitatea lui.
Într-un mediu rapid și competitiv din zilele de azi reprezintă o preocupare majoră a industriei de
construcții nevoia de eficientizare a proceselor pentru a economisi timp și bani, sistemele de beton
super fluid permitând astfel de economii. Folosirea agregatelor reciclate în fabricarea betonului
autocompactant este benefică atât din punct de vedere a sustenabilității cât și pentru a reduce
impactul depozitării deșeurilor din industriile de construcții asupra mediului.
Ipotezele de lucru de la care s-a pornit au fost acelea că într-un timp de amestecare mai lung al
agregatelor, ele genereaza mai multe particule fine, care ar influența lucrabilitatea betonului. Testele
reologice ne ajută să descoperim comportamentul în timp al betonului autocompactant, folosind
varianta studiului mortarului echivalent fără agregatele grosiere sau pasta de mortar.
Reologia este știința ce studiază interdependența între solicitările mecanice, răspunsul corpurilor și
proprietățile acestora. Această știință stabilește modelele matematice care descriu comportamentul
corpurilor supuse la solicitări. Reologia materiei se caracterizează în principal prin doi parametri:
rezistența la curgere și vâscozitatea plastică.
În primul capitol sunt prezentate obiectivele generale ale lucrării, descoperirea betonului
autocompactant și avantajele lui în dezvoltarea industriei construcțiilor.
Capitolul doi conține aspecte generale despre betonul autocompactant, agregatele reciclate, ciment
și superplastifiant. În anul 1986, prof. Okamura, de la Universitatea Ouchi din Japonia a conceput
acest tip de beton într-o perioadă în care forța de muncă calificată era în cantități limitate,
provocând dificultăți în industriile legate de beton. Betonul autocompactant poate fi utilizat pentru
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turnarea secțiunilor care conțin multă armature, a locurilor în care nu pot fi accesate vibratoarele
pentru compactare și în forme de cofrare care altfel ar putea fi imposibil de turnat. Costul relativ
mare al materialului utilizat în astfel de beton continua să impiedice utilizarea pe scară largă a
acestuia.
Tot în capitolul doi sunt prezentate date despre cimentul și superplastifiantul folosit în programul
experimental, cât și noțiuni generale despre agregatele reciclate. Datorită faptului că agregatele
naturale (pietriș, nisip și piatră spartă) sunt resurse ne-regenerabile esențiale care pot fi utilizate
pentru infrastructuri și inginerie civilă, s-a implementat programul SARMa în mai multe state
europene, având unul dintre obiectivele principale valorificarea unor părți din deșeuri și
reintroducerea lor în ciclurile productive, sub formă de produse sau materii prime. Reciclarea
deșeurilor din construcții și demolări oferă oportunități importante pentru reducerea necesarului de
terenuri pentru haldare, evitarea supra-consumului de resurse de agregate naturale ne-regenerbile,
prin introducerea de materiale alternative si suplimentare pe piața agregatelor, crearea de noi
posibilități de afaceri prin reciclarea deșeurilor.
Capitolul trei conține procedeul experimental. De-a lungul cercetării s-au conceput 18 paste de
mortar având în componentă particule fine mai mici de 0,125 mm de agregat natural și agregat
reciclat. În vederea observării mai bune a diferenței între cele două tipul de particule fine, s-au
realizat paste de mortat cu un raport apă/ciment egal cu 0,4 și un dozaj de superplastifiant de 0,12,
atât în cazul particulelor fine naturale cât și în cazul particulelor fine reciclate. Proporțiile de
introducere a particulelor fine au fost de 20,30, 40 respectiv 45% din volumul total al pastei.
Pornind de la premiza că într-un timp mai mare de amestecare se generează mai multe particule fine
care influențează lucrabilitatea betonului, agregatele au fost supuse unui amestec de 5 și 15 min în
malaxor, apoi extrase particulele fine mai mici de 0,125 mm pentru producerea pastei de mortar.
În acest sens, am avut 3 tipuri de paste cu timpi diferiți de amestecare al agregatelor si cu procentaje
diferite de particule fine incorporate.
Minutul zero este considerat momentul în care s-au adăugat particulele fine împreuna cu apa extra
în mixer, amestecându-se timp de 1 minut apoi fiind lăsate în stare de repaus pentru a se hidrata.
Cantitatea de apă extra s-a determinat în funcție de procentajul de absorbție al agregatelor în decurs
de 24 de ore. Minutul 10 este alocat adăugării de ciment, urmând la minutul 11 apa, minutul 12
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superplastifiantul, de la minutul 13 până la minutul 14 pasta este lăsată în stare de repaus, iar apoi
amestecată pentru încă un minut.
Asupra pastei de mortar s-au efectuat testele reologice, cu ajutorul reometrului Viskomat NT
special conceput pentru pasta de mortar cu agregate de dimensiuni până în 2 mm, la minutul 32 si
52 de la contact. Înaintea efectuării testului de rezistență la curgere, pasta de mortar s-a lăsat în stare
de repaus, urmând testul de vâscozitate plastică. Ambele teste au fost efectuate de două ori asupra
fiecărei probă.
După efectuarea fiecărui test în parte, s-au procesat datele și a urmat prelucrarea lor în vederea
obținerii unor rezultate cât mai relevante.
În urma cercetărilor efectuate de diferiți autori, atât betonul autocompactant proaspăt cât și mortarul
autocompactant pot fi modelaț ca un fluid viscoelastic cu un model care descrie rezistența la curgere
și vâscozitatea plastică. Există diferite modele care corelează aceste proprietăți, dar modelul
Bingham este unul dintre cele mai simple și mai acceptate. În schimb pasta de mortar se încadreză
în modelul Modified-Bingham având ecuația de modelare 𝜏 = 𝜏! + 𝜇𝛾 + 𝒸𝛾 ! . Valorile rezistenței
la curgere și a vâscozității plastice au fost calculate la o viteză constantă de 100 rpm.
În cazul pastei de mortar cu o fracție volumică de 40% după un amestec al agregatelor de 15 minute
s-a observat o pierdere totală a caracteristicii de autocompactare și o imposibilitate de efectuare a
testelor, datorită absorbției ridicate de apă ale particulelor fine.
S-a observat o diferență relevantă în cazul pastei de mortar cu particule fine naturale încorporate în
comparație cu pasta de mortar având încorporat particule fine reciclate.
Pentru o și mai bună analiză a înfluenței particulelor fine, s-a preparat o monstră de mortar
folosindu-se nisip convențional, încorporându-se, în proporții de 10,69% și 12,21%, particule fine
mai mici de 0,063mm.
După prepararea monstrelor, s-au turnat 2 prisme a câte 40×40×160 mm și s-a efectuat testul pentru
determinarea timpului de lucrabilitate a mortarului conform normativului EN 1015-9.
Timp de 24 ore, monstrele au fost păstrate în camera climatică, iar apoi au fost supuse determinării
rezistenței la compresiune și inflexiune dupa 1, 3,7 respectiv 28 zile.
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Asupra unei cantități de 50g de particule fine s-a realizat, într-un alt laborator al Universității Da
Coruna, analiza termogravimetrică ce constă în măsurarea schimbărilor masei unei probe pe
parcursul unui program de termperatură bine stabilit într-o atmosferă controlată.
La finalul prelucrării tuturor datelor s-a putut constanta faptul că un timp mai mare de amestecare
generează mai multe particule fine care influențează negativ lucrabilitatea pastei de mortar
autocompactant. Încorporarea particulelor fine reciclate până în proporții de 30% și un timp de
amestec al mortarului mai mic de 15 minute nu are influențează comportamentul reologic al pastei
de mortar autocompactant. Pastele de mortar cu o fracție volumică mai mare de 40% și-au pierdut
automat caracteristicile de autocompactare și imposibilitatea realizării testelor reologice.
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TABLE OF CONTENT

CHAPTER 1: INTRODUCTION AND OBJECTIVES ............................................................................ 9
1.1 Introduction: general concepts ..................................................................................................................... 9
1.2 General objective ......................................................................................................................................... 9
CHAPTER 2: STATE OF ThE ART ................................................................................................. 10
2.1 Self-compacting concrete ........................................................................................................................... 10
2.2 Recycled aggregates ................................................................................................................................... 11
2.3 Cement ....................................................................................................................................................... 14
2.4 Superplasticizer .......................................................................................................................................... 16
CHAPTER 3: Materials and experimental procedures ................................................................. 17
3.1 Materials preparations ................................................................................................................................ 17
3.2 Granulometry determination ...................................................................................................................... 17
3.3 Mixing procedure ....................................................................................................................................... 20
3.4 Results ........................................................................................................................................................ 21
3.4.5 TGA Analysis.......................................................................................................................................... 49
3.4.6 Yield stress comparison .......................................................................................................................... 50
CHAPTER 4: Conclusions ............................................................................................................ 51
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CHAPTER 1: INTRODUCTION AND OBJECTIVES
1.1 Introduction: general concepts
Based on the rule that a concrete is made out of a liquid phase (paste) and a solid phase
(aggregates with fixed gravel/sand ratio), the concrete self-compacting properties come
fundamentally from those of the paste. The present paper reveals the rheological behavior of the
paste and its influences in concrete manufacturing.
For several years, beginning in 1983, the problem of durability of concrete structures was a
major topic of interest in Japan. To make durable concrete structures, sufficient compaction by
skilled workers is required. However, the gradual reduction in the number of skilled workers in
Japan’s construction industry had led to a similar reduction in the quality of construction work. One
solution for the achievement of durable concrete structures independent of the quality of
construction work is the employment of self-compacting concrete. [1]
To achieve self-compacting concrete, investigating the characteristics of mortar paste,
aggregates, cement, additives, is absolutely necessary.
Rheology is the study of the flow of matter, primarily in a liquid state, but also as “soft
solids” or solids under conditions in which they respond with plastic flow rather than deforming
elastically in response to an applied force. It is a branch of physics, which deals with the
deformation, and flow of materials, both solids and liquids. [2]
1.2 General objective
The primary purpose of this research is to obtain the rheological behavior of fresh mortar
paste, containing water, cement and fine aggregates smaller than 0,125 mm, in order to understand
its influence on self-compacting mortar and also to analyse its basic mechanical properties. The
fines aggregates used are fine natural aggregates (FNA) and fine recycled aggregates (FRA).
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CHAPTER 2: STATE OF ThE ART
2.1 Self-compacting concrete
Self-compacting concrete is an innovative material that can flow through and fill the gaps of
reinforcements, corners of molds, and voids of rock blocks without any need for vibration and
compacting during the placing process, which improves the overall efficiency of concrete
construction projects. The key requirements for SCC are high flow ability without the segregation
of aggregate during placement. [3]
Ordinarily, concrete is a dense, viscous material when mixed, and when used in
construction, requires the use of vibration or other techniques (known as compaction) to remove air
bubbles (cavitation), and honeycomb-like holes, especially at the surfaces, where air has been
trapped during pouring. This kind of air content is not desired and weakens concrete if left.
However it is laborious and takes time to remove by vibration and improper or inadequate vibration
can lead to undetected problems later. Additionally some complex forms cannot easily be vibrated.
Self-compacting concrete is designed to avoid this problem, and not require compaction,
therefore reducing labor, time and a possible source of technical and quality control issues. [4]
Okamura proposed the necessity of this type of concrete, in 1986. Studies to develop self-
compacting concrete, including a fundamental study on the work-ability of concrete, have been
carried out by Ozawa and Maekawa at the University of Tokyo.
The three properties that characterize a concrete as self-compacting are:
• Flowing ability - the ability to completely fill all areas and corners of the formwork into
which it is placed;
• Passing ability - the ability to pass through congested reinforcement without separation of
the constituents or blocking;
• Resistance to segregation - the ability to retain the coarse components of the mix in
suspension, in order to maintain a homogeneous material.
These properties must all be satisfied in order to design an adequate SCC, together with other
requirements including those for hardened performance.
SCC was first developed in Japan in 1988 in order to achieve durable concrete structures by
improving quality in the construction process. It was also found to offer economic, social and
environmental benefits over traditional vibrated concrete construction. Research and development
work into SCC in Europe began in Sweden in the 1990s and now nearly all the countries in Europe
conduct some form of research and development into the material.
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2.2 Recycled aggregates
Concrete is the most used material in building and infrastructure construction, having the
main raw materials aggregates with a proportion of 60-80% in volume. This represents a huge
demand of materials that is satisfied mostly by natural sources. At the same time, the demolition
and repair works produce large amounts of construction and demolition waste. In this context, the
use of construction and demolition waste debris as aggregates in concrete production is a logical
step with both economic and environmental benefits that has been growing in the last two decades.
Research on construction and demolition waste has reached some consensus concerning the
homogeneity and acceptable quality of coarse recycled aggregates (CRA) from crushed concrete.
Kou and Poon [5] tried to demonstrate the feasibility of utilizing fine and coarse recycled
aggregates with rejected fly ash and Class F fly ash for self-compacting concrete. The mixture
contained Portland cement, two types of fly ash (fine fly ash and rejected fly ash), coarse recycled
aggregates with nominal sizes of 20 mm and 10 mm, river sand with a fineness modulus of 2.11 as
the fine natural aggregates, recycled aggregates with a particle size of<5mm was used as fine
recycled, superplasticizer and a viscosity agent. They prepared three series of SCC mixtures with
different fine recycled aggregate contents and water-to-binder (W/B) ratios, which were mixed for 5
minutes in a laboratory mixer, and before casting, a variety of tests were performed on them to
determine their fresh properties, including leakage rate, flow time, segregation resistance, ratio
blocking and wet density. For each concrete mixture fifteen cubes were cast for the determination
of compressive strength, seventeen cylinders were cast for the determination of splitting tensile
strength and the resistance to chloride-ion penetration. Furthermore, three prisms were cast for
measuring the drying shrinkage. After casting, all the specimens were covered with plastic sheets
and water saturated burlaps before being air cured in the laboratory for 24 h. The compressive
strength test was carried out on the concrete specimens at the ages of 1, 4, 7, 28 and 90 days while
the splitting tensile strength test was carried out on the concrete specimens at the age of 28 days.
The chloride penetrability of concrete was determined at the ages of 28 and 90 days.
The results show that the both coarse and fine recycled aggregates can be used for SCC production,
and with increasing fine recycled aggregate content the slump flow and blocking ratio of the RA-
SCC mixtures increased, the compressive and tensile splitting strengths of the RA-SCC mixtures
prepared without the addition of fly ash decreased, the maximum compressive and tensile splitting
strength were achieved by using 25–50% fine recycled aggregates as a replacement of river sand,
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the resistance to chloride ion penetration and the drying shrinkage of the RA-SCC mixtures
increased.
Starting from other research in the field, more researchers from University of A Coruna and
University of Lisbon studied the effect of incorporating fine recycled aggregates on the rheology of
self-compacting concrete over time (at 15, 45 and 90 min). The fine fraction of the natural
aggregates was replaced at 0%, 20%, 50% and 100% with recycled sand. In their SCC mixture was
used Portland cement, limestone filler, three types of aggregates (the coarse fraction was natural
limestone gravel, fine aggregates were natural limestone sand that was partially replaced by
recycled sand) and superplasticizer. By approaching the equivalent mortar, it was possible to make
a suitable SCC composition, this mixture being tested on a complete scale of the concrete, obtaining
a SCC with acceptable flow results, but high values in the test with the V funnel. The mini-cone and
mini-funnel tests were performed on the mortar, observing a higher spreading in lower replacement
reports. In the results of the mini-funnel test there is a decrease in time and with the replacement
ratio, being impossible to carry out the test in the case of the mixture with 100% recycled material
due to the loss of workability. Tests on SCC's fresh behavior were performed, observing that for
mixtures with 50% and 100% FRA, they completely lost the characteristics of a self-compacting
concrete after 90 min. Both properties, passing ability and filling ability, deteriorated over time for
all replacement ratios and the reference concrete. Nevertheless, this reduction increased with the
replacement ratio. The compressive strength decreases with incorporation of recycled sand. The
mix with 20% recycled sand only showed a reduction of 8% of compressive strength at 28 days,
relative to the reference concrete, whereas the one with 100% recycled sand exhibited a reduction
of 47%, similar to the effect detected in the mortar. The mix with 20% replacement did not show
any loss of SCC characteristics and the reduction of compressive strength was less than 10%.
Therefore, this replacement ratio of natural sand with recycled sand is considered feasible for the
production of SCC.
Regarding the rheological characteristics of self-compacting concrete using recycled
aggregates, there have been several studies that have revealed its influence on concrete. In this case,
Erhan Güneyisi, Mehmet Gesoglu [6] used recycled aggregates, as coarse and fine recycled
aggregates, in SCC mixtures; CRCA was substituted for 0%, 50% and 100% natural coarse
aggregates. In each series of mixtures, the natural fine aggregate was replaced with FRCA as 0%,
25%, 50%, 75% and 100%. In their work, Herschel-Bulkley and modified Bingham models were
adopted to describe the rheological behavior of SCC with RCA indicating a non-linear and shear
thickening behavior due to lower yield stress close to zero. Bingham model is not applicable for
SCC, which should not be ignored in the prediction of shear stress of fresh concrete to avoid
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breaking of the mixer, pump or pipes. The replacement levels of CRCA and FRCA used in SCC
mixtures improve the self-compactibility characteristics of the concretes.
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2.3 Cement
Cement is a binder, a substance used for construction that sets, hardens and adheres to
other materials, binding them together. It is used with fine aggregates to produce mortar for
masonry, or with sand and gravel aggregates to produce concrete.
Cements used in construction are usually inorganic, often lime or calcium silicate based, and can be
characterized as being either hydraulic or non-hydraulic, depending upon the ability of the cement
to set in the presence of water.
Portland cement is the most common type of cement in general use around the world as a basic
ingredient of concrete, mortar, stucco, and non-specialty grout. It was developed from other types
of hydraulic lime in England in the mid 19th century, and usually originates from limestone. It is a
fine powder, produced by heating limestone and clay minerals in a kiln to form clinker, grinding the
clinker, and adding 2 to 3 percent of gypsum.
Several types of Portland cement are available. The most common, called ordinary Portland cement
(OPC), is grey in color, but white Portland cement is also available. Its name is derived from its
similarity to Portland stone, which was quarried on the Isle of Portland in Dorset, England. Joseph
Aspdin, who obtained a patent for it, in 1824 named it. However, his son William Aspdin is
regarded as the inventor of "modern" Portland cement due to his developments in the 1840s.
The European norm EN 197-1 defines five classes of common cement that comprise Portland
cement as a main constituent. These classes differ from the ASTM classes.
• CEM I Portland cement: comprising Portland cement and up to 5% of minor additional
constituents
• CEM II Portland-composite cement: Portland cement and up to 35% of other single
constituents CEM III Blast furnace cement: Portland cement and higher percentages of blast
furnace slag
• CEM IV Pozzolanic cement: Portland cement and up to 55% of pozzolanic constituents
• CEM V Composite cement: Portland cement, blast furnace slag or fly ash and pozzolana.
The cement used for my project is CEM I 52,5 N-SR 5 containing reducer of Cr (VI), with
guarantees a content of Cr (VI) soluble in water less that 0,0002%.
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Figure 1 Cement CEM I 52,5 N-SR 5
The main fields of application are:

• Concrete subjected to corrosion of armor by chlorides of marine origin.
• Pre-stressed concrete including structural prefabricated.
• Reinforced concrete.
• Reinforced concrete prefabricated structural elements.
• Concrete exposed to chemical aggressiveness, acid waters, sulfates, etc.
• Concrete dams, when an addition is added to the concrete in sufficient quantity.
• Concreting in cold weather.
• Concrete for quick emergency repairs.
• Reinforced concrete foundations.
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2.4 Superplasticizer
Concrete is a composite material in which aggregates are bound by hydrated cement paste. The
quantity of water demanded for the reaction of hydration represents about 25% of the mass of
cement. However, in order to obtain a flowing concrete, is required much more water (about
double), which in the long term, it evaporates, leaving voids in the concrete. The associated porosity
decreases both the mechanical strength and the durability. [7]
For this reason, superplasticizers, also known as high range water reducers, are of interest. It are
chemical admixtures used where well-dispersed particle suspension is required. These polymers are
used as dispersants to avoid particle segregation (gravel, coarse and fine sands), and to improve the
flow characteristics (rheology) of suspension such as in concrete applications. With relatively low
dosage (0,15-0,3% by cement weight) they allow a water reduction up to 40% for the same
workability.
Nowadays, superplasticizers are most widely used in Japan, where it is estimated that almost no
concrete is produced without it. [7]
The superplasticizer used in this research is MasterEase 3850, manufactured based on the new
technology of PAE polymers exclusive of BASF Construction.
Figure 2 Superplasticizer MasterEase 3850
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CHAPTER 3: Materials and experimental procedures
In the experimental procedure, a series of 18 pastes were made in order to discover the effects of
fine aggregates generated through process mixing time on the rheological behavior of mortar paste.
W/C ratio and super plasticizer dosage were kept constant in every paste but the percentage of fines
origins were changed, using 20, 30,40 and 45 solid volume fraction.
3.1 Materials preparations
The first step was to dry all aggregates, for 24 hours, in special electric equipment. After that the
aggregates were sieved through 0,125mm sieve and kept in plastic bags, till the moment of use.
Figure 3 Drying oven Figure 4 Stored FNA and FRA
3.2 Granulometry determination
At the base of the mixing process of the paste is the mixing process of the mortar, which influences
its later behavior. In the case of the mortar, a time span was used to hydrate the particles, while the
actual mixing time of all the components is different.
Figure 5 5 minutes mixing protocol
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Figure 6 15 minutes mixing protocol
According to several authors, during the mixing time, the aggregates could break what would cause
a larger generation of fine particles smaller than 0,125 mm. Due to this fact, the workability of the
mortar would decrease, especially in self-compacting recycled concrete (SRC).
Considering that two different mixing times will be used to prepare the mortar, we have come to the
conclusion that the same thing should be done only with aggregates. In that case, a total of 30kg
natural sand and 25kg recycled sand was mixed for 5, respectively 15 minutes. The quantities were
chosen by the fact that the same amount would be used for preparing the mortar with 45% volume
fraction. Using a sample splitter, we managed to obtain the 250g needed for measuring the
granulometry of sands.
Figure 7 Sample splitter Figure 8 The coning and quartering method
Figure 9 Coning and quartering natural sand

Figure 10 Particle size distribution

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The results of the granulometry test have shown us that indeed, during the mixing of the mortar
components, the aggregates break, generating more fine particles smaller than 0,125 mm.
Chart 1 Particle size distribution of Recycled Sand
Chart 2 Particle size distribution of Natural Sand
The fines origins of natural sand is 15,39% and the fines origins of recycled sand is 16,25%.
Starting from these numbers, we can see an increase of 1,44% and 6,4% in the sand mixed for 5
minutes and 3,08%, respectively 6,29% in 15 minutes mixed sand.
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3.3 Mixing procedure
According to Evangelista, L., De Brito, J., [8] the water absorption of FRA is higher than that of
FNA, which is the main physical characteristic between FRA and FNA, that differs the most. In this
case, at the beginning of the mix, we decided to hydrate the particles in order to be sure that the rest
of water to enter in contact with the cement, and keep the water/cement ratio constant. That moment
is considered the 1’ of the mix protocol. For 9 minutes, the fines are left to hydrate; at the 10’ we
add the cement, followed at 11’ by the rest of water (W1) and at 12’ by superplasticizer + water
(W2). After this process is over, we put the paste into the Viskomat NT, rheometer for mortar and
paste. It is a versatile rotational viscometer, used for determine the workability of fine-grained
buildings materials such as cement paste, mortar, fine concrete, plaster etc., with a maximum
particle size of 2 mm.
Figure 11 Mortar Paste Mixer Figure 12 Viscometer Viskomat NT
The rheology measurement starts at 32’ from the contact with Stress Grow Test (SGT) and followed
with Flow Curve Test (FCT). Before starting the measurement, at 26’ we mix with a spoon inside
the paste, letting at rest for 5 minutes. First after the SGT is finished, we start the FCT but not
before we mix again with a spoon the paste.
By adjusting the extreme paste, 0,2 volume fraction natural sand and 0,45 volume fraction recycled
sand, we managed to obtain two series of 9 mortar paste, using FRA and FNA.
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Having the data measured, we analyse and process it afterwards, in order to obtain the graphic for
each test.
3.4 Results
In order to fill the container of rheometer and to have a homogeneous mortar paste, I prepared 1,5l
of mortar paste, with 0,4 w/c ratio and 0,12 superplasticizer dosage. All the mixes were created
having in account the water absorption of aggregates and the time upon which the aggregates were
subjected.
3.4.1 Paste with 0,2 Solid Volume Fraction
The proportions listed in Table 1 are characteristic of the mortar paste with 0,2 solid volume
fraction, which aggregates were not subjected any mixes before.
Material Weight (g)
Cement 1964,63
Water 777,74
Fines origin 182,16
Super 11,79
Total 2936,33
Table 1 Natural Sand, 0,2 solid volume fraction, 0’mix
Underneath are shown the results of stress grow test, in which we can observe that the maximum
torque from first measurement is 3,96 N.mm and from the second one is 5,30 N.mm.
Chart 3 Stress grow results-NS, 0,2 Solid Volume Fraction, 0’ mix

PASTE
Chart 4 Flow curve results-NS, 0,2 Solid Volume Fraction, 0’ mix
In order to describe the rheological behavior of SCC paste, the modified Bingham model was used,
of which equation is:
𝜏 = 𝜏! + 𝜇𝛾 + 𝒸𝛾 !
At 100rpm speed, the value of viscosity is 0,08 N.mm.min in both measurements and the values of
yield stress are 0,142 N/mm2 and 0,149 N/mm2 .
Table 2 contains the material quantities for the paste whose aggregates were mixed during 5’,
before sieving it. The amount of fines was determinated taking into account the fines generated,
which was calculated after the sand was subjected to granulometry determination.
Material Weight (g)

Cement 1956,307
Water 774,571
Fines 198,364
Super 11,738
Total 2940,98
Table 2 Natural Sand, 0,2 solid volume fraction, 5’ mix
As in the previous case, we can see the maximum torque, which is 5,71 N.mm in the first
measurement, followed by 6,75 N.mm in the second one.
PASTE
Chart 5 Stress grow results-NS, 0,2 solid volume fraction-5’ mix
In this case, the viscosity resulted at a speed of 100rpm is 0,12 N.mm.min and the value of yield
stress is 0,1415 N/mm2 in first measurement, followed by 0,1 N.mm.min and 0,512 N/mm2 .
Chart 6 Flow curve results-NS, 0,2 Solid Volume Fraction, 5’ mix
PASTE
Material Weight (g)

Cement 1946,91
Water 770,99
Fines 216,65
Super 11,68
Total 2946,23
Like other two tables showed us the mix proportions, Table 3 contains the quantities of materials
we need in case of paste mortar with aggregates subjected to 15’ mix.
Due to the fact that after 15’ mix the sand will generate more fines than in the previous case, a
higher quantity will be used.
We can see that the maximum torque in first measurement is 5,14 N.mm and, repeating the test after
20 minutes, it increased with 0,98 N.mm, reaching value 6,12 N.mm in the first 10 seconds from the
start.
The flow curve test is presented in Chart 8 and it shows us that the viscosity is constant in both
cases, 0,1 N.mm.min at a constant speed of 100rpm, but the yield stress values are 0,1409 N/mm2 in
first measurement and 0,1469 N/mm2 in the second one.
PASTE
Chart 8 Flow curve results-NS, 0,2 solid volume fraction-15’ mix
As long as mortar paste with recycled aggregates has been made, I will continue to present the
results obtained after the rheological test were made. In this case, Table 4 will present the material
quantities needed for the same amount of paste, respectively 1,5l.
Material Weight (g)

Cement 1958,31
Water 785,16
Fines origin 154,78
Super 11,75
Total 2910,01
Table 4 Recycled Sand, 0,2 solid volume fraction, 0’mix
From Chart 9 we would see that the values of stress grow test are higher in case of paste with FRA.
The maximum torque is 6,48 N.mm in the first measurement and 7,57 N.mm in the second
measurement, with an average of 5,40 N.mm, respectively 5,16 N.mm.
PASTE
Chart 9 Stress grow results-RS, 0,2 solid volume fraction-0’ mix
In the next case, from Chart 10 we can see that the viscosity, for 100rpm speed, remains constant
for both measurements, 0,14 N.mm.min but the value of yield stress is decreasing from 0,1573
N/mm2 to 0,1407 N/mm2.
Chart 10 Flow curve results-RS, 0,2 solid volume fraction-0’ mix
PASTE
Material Weight (g)

Cement 1921,597
Water 774,785
Fines 211,655
Super 11,530
Total 2919,57
Table 5 will present the quantities of material necessary for paste with aggregates subjected at 5’
mix before sieving.
The maximum torque observed here is 11,28 N.mm in first measurement, respectively 12,74 N.mm
in second measurement, obtain in the first 10 seconds of the test.
If we compare the results from 0’ mix to the 5’ mix, we can observe a big difference, one that, in
the natural sand case, is not so obvious.
Analyzing Chart 12, we can see that, for a constant speed of 100rpm, the value of viscosity will be
constant in both measurements, equal with 0,14 N.mm.min, but with a higher yield stress value,
compared with previous paste, which is 0,1909 N/mm2 in first measurement and 0,177 N/mm2 in
the second measurement.
PASTE
Table 6 will present the quantities of material necessary for paste with aggregates subjected at 15’
mix before sieving.
Material Weight (g)

Cement 1918,67
Water 773,96
Fines 216,18
Super 11,51
Total 2920,33
The values for stress grow test, obtained from measurements, are presented in Chart 13 followed by
Chart 14, presenting the values for flow curve test.
The maximum torque in stress grow is 11,43 N.mm followed by 12,56 N.mm, with an average of
10,47 N.mm and 9,86 N.mm.
In case of viscosity, we can see that remains the same in both measurements and it is equal with
0,12 N.mm.min for 100rpm speed. The values of yield stress being 0,198 N/mm2 and 0,787 N/mm2 .
PASTE
PASTE
3.4.2 Paste with 0,3 Solid Volume Fraction
Table 7 contains the quantities for the next type of paste, with 30% fines, w/c=0,4 and
superplasticizer dosage 0,12.
Material Weight (g)

Cement 1897,78
Water 752,27
Fines 312,28
Super 11,39
Total 2973,71
Chart 15 presents the recorded values of stress grow test, showing that the maximum torque is 4,76
N.mm in first measurement case and 5,71 N.mm in second measurement case, with an average of
3,64 N.mm and 3,60 N.mm.

PASTE
From Chart 16 we can see that the value of viscosity is 0,12 N.mm.min, in both cases, at 100rpm
speed but the value of yield stress is higher in the second measurement, reaching the value of
0,1488 N/mm2, compared with 0,1416 N/mm2.
Table 8 lets us know the amounts of each material used for the mortar paste made with fines
aggregates subjected to 5’ mix before using it.
Material Weight (g)

Cement 1884,036
Water 747,030
Fines 339,027
Super 11,304
Total 2981,40
Chart 17 reveals the maximum torque registered in first measurement, 3,70 N.mm, and in second
measurement, 4,37 N.mm, with an average of 3,02 N.mm and 2,81 N.mm.
PASTE
The values of viscosity in this case are 0,14 N.mm.min in first measurement, and 0,12 N.mm.min in
the second measurement, with an yield stress point equal with 0,1115 N/mm2 and 0,1269 N/mm2.
PASTE
Material Weight (g)

Cement 1868,63
Water 741,16
Fines 369,02
Super 11,21
Total 2990,01
Table 9 presents the materials needed for paste with FNA subjected to 15’ mix before using.
Chart 19 shows us that the maximum torque in first measurement is 9,12 N.mm and in the second
measurement 10,40 N.mm, with an average of 8,13 N.mm and 7,35 N.mm.
Chart 20 reveals us that the viscosity is 0,12 N.mm.min in first measurement and 0,1 N.mm.min in
the second measurement, with a yield stress value at 100rpm of 0,20 N/mm2 in first measurement,
and 0,22 N/mm2 in second measurement.
PASTE
From Table 10 will discover the materials needed for paste made with 0,3 solid volume fraction of
fine recycled aggregates not subjected to a mix before.
Material Weight (g)

Cement 1886,95
Water 764,99
Fines 265,33
Super 11,32
Total 2928,59
Chart 21 will give us the values of maximum torque in each measurement and the average.
In this case we have 13,88 N.mm and 17,11 N.mm for maximum torques, followed by 12,78 N.mm
and 14,02 N.mm as averages torques.
From Chart 22 we discover the values of viscosity, 0,12 N.mm.min and 0,10 N.mm.min, and yield
stress, 0,249 N/mm2 and 0,256 N/mm2
PASTE
Chart 22 Chart 23 Flow curve results-RS, 0,3 solid volume fraction-0’ mix
PASTE
Material Weight (g)

Cement 1827,101
Water 748,070
Fines 358,043
Super 10,963
Total 2944,18
Table 11 Recycled Sand, 0,3 solid volume fraction, 5’ mix
In Table 11 we have the quantities used for paste with 0,3 solid volume fraction of fine recycled
aggregates subjected to 5’ mix before using it.
Chart 24 shows us that the maximum torque, which is measured in the first 10 seconds from the
start, is 65,11 N.mm and 68,07 N.mm, followed by the average torques, 65,42 N.mm and 61,07
N.mm, measured between second 30 and second 50.
The viscosity, in this case, is 0,06 N.mm.min and 0,04 N.mm.min, lower than the previous example,
but with a value of yield stress higher, 0,364 N/mm2 respectively 0,360 N/mm2.
PASTE
Table 15 shows us the quantities necessary for paste made with 0,3 solid volume fraction of fine
recycled aggregates, subjected at 15’ mix before used it.
Material Weight (g)

Cement 1822,40
Water 746,74
Fines 365,32
Super 10,93
Total 2945,40
The maximum torque in this case is 37,32 N.mm and 48,23 N.mm, with an average of 37,70 N.mm
and 40,63 N.mm, which is showed in Chart 26.
Chart 27 reveals the values of viscosity, 0,08 N.mm.min and 0,06 N.mm.min, with a value of yield
stress equal with 0,31 N/mm2, respectively 0,35 N/mm2, at 100rpm speed.
PASTE
PASTE
3.4.3 Paste with 0,4 solid volume fraction
Table 13 will reveal the quantities used for preparing paste with 0,4 solid volume fraction of FRA,
without being subjected to any mix before.
Material Weight (g)

Cement 1791,79
Water 738,09
Fines 412,74
Super 10,75
Total 2953,37
The value of maximum torque is 78,93 N.mm in first measurement, 90,35 N.mm in second
measurement, with an average of 81,10 N.mm, respectively 78,70 N.mm, presented in Chart 28.
Chart 29 is showing us the values of viscosity and yield stress, at a speed of 100rpm.
In this case, we have 0,12 N.mm.min in first measurement, 0,08 N.mm.min in second measurement,
and yield stress equal with 0,452 N/mm2, respectively 0,437 N/mm2.
PASTE
Underneath, Table 14 shows the quantities used for preparing the paste with FRA subjected to 5’
mix before using it.
Material Weight (g)
Cement 1704,924
Water 713,529
Fines 547,312
Super 10,230
Total 2975,99
From Chart 30 we can see that the maximum and average torque obtained in first 10 seconds are:
- First measurement: 233 N.mm maximum torque, 222,39 N.mm average torque;
- Second measurement: 210,10 N.mm maximum torque, 277,61 N.mm average torque.
PASTE
PASTE
3.4.4 Paste with 0,45 solid volume fraction
Table 15 contains the quantities of materials used in preparation of paste with 0,45 solid volume
fraction of fine natural aggregates.
Material Weight (g)

Cement 1751,92
Water 696,68
Fines 596,17
Super 10,51
Total 3055,28
- First measurement: 25,94 N.mm maximum torque, 25,32 N.mm average torque;
PASTE
The values of viscosity and yield stress are extracted from Chart 33, at a constant speed of 100rpm
we have:
- Viscosity in first measurement: 0,1 N.mm.min;
- Yield stress in first measurement: 0,443 N/mm2;
- Viscosity in second measurement: 0,08 N.mm.min;
- Yield stress in second measurement: 0,423 N/mm2.
In Table 16 we have the quantities used for preparing paste with 0,45 solid volume fraction of NFA
subjected to 5’ mix before mixing it.
Material Weight (g)
Cement 1727,86
Water 687,51
Fines 643,00
Super 10,37
Total 3068,74
Maximum and average torque are presented in Chart 34:

PASTE
PASTE
we have:
Table 17 contains the quantities of materials used in preparation of paste with 0,45 solid volume
fraction of fine natural aggregates, subjected to 15’ mix before usage.
Material Weight (g)

Cement 1701,25
Water 677,37
Fines 694,79
Super 10,21
Total 3083,62
PASTE
we have:
3.4.5 The workability of mortar
The workability of the mortar was determined according to EN 1015-9. In the mortar
composition was used standardized sand which had the fines particles<0,063 mm replaced with fine
natural aggregates and fine recycled aggregates, in proportions of 10,69% and 12,21%.
The mixing procedure was exactly the same like in the paste and mortars mixes. I prepared
1,9l of mortar in order to make the workability test and to fill, for each mortar, two 40×40×160 mm
prisms.
PASTE
Figure 14 Specimens prepared for workability test
By interpolating, we obtain the time in which the mortar reaches the resistance of 0,5
N/mm2. The results are:
• NS-10,69%: 5h34’
• NS-12,21%: 5h35’
• RS-10,69%: 5h31’
• RS-12,21%: 5h28’
Figure 15 Cast specimens and hydraulic press
After 24h, the samples were detached and 2 of each mortar were used to determine the
inflexion and compressive strength at 1 day. The procedure was repeated after 3, 7 and 28 days.
PASTE
Inflexion strength [MPa]

Age [days] NS-10,69 NS-12,29 RS-10,69 RS-12,21
1 6,31 6,59 4,75 4,79
3 6,14 6,62 4,29 4,31
7 7,64 8,35 5,93 5,67
28
Table 18 Inflexion strength [MPa]

Compression strength [MPa]
Age [days] NS-10,69 NS-12,29 RS-10,69 RS-12,21
1 33,62 31,50 24,54 24,63
3 50,86 49,45 41,42 39,51
7 56,81 58,25 47,72 46,82
28
Table 19 Compression strength [MPa]
PASTE
3.4.5 TGA Analysis
The fines used in the process of mortar paste making were subjected to a thermogravimetric
analysis (TGA) at Edificio dos Servizos Centrais de Investigación - Campus de Elviña s/n.
Thermogravimetric Analysis is a technique in which the mass of a substance is monitored as

a function of temperature or time as the sample specimen is subjected to a controlled temperature
program in a controlled atmosphere. [9]
0.00
100
DSG (%/min)
-0.25
95 -0.50
TG (%)
90
FRA-TGA
FRA_FLL-TGA
FRA-DSG
FRA_FLL-DSG
85
0 100 200 300 400 500 600 700 800 900 1000
Temperature (ºC)
Chart 38 TGA Analysis of FRA

Chart 38 shows us the weight losses of FRA in percentage, from temperature 0 to 900. This
loss is typically caused by chemical reactions (decomposition and loss of water of crystallization,
combustion, reduction of metal oxides) and physical transitions (vaporization, evaporation,
sublimation, desorption, drying). [10]
The values of mass loss are showed in table 20:
Temperature FRA_FLL FRA Diff

300 97,576 98,389 -0,81327
600 94,106 96,103 -1,99704
900 87,428 91,086 -3,65758
Table 20 Mass Loss of FRA
PASTE
3.4.6 Yield stress comparison
Chart 39 Comparison between yield stress values of paste with FNS
Chart 40 Comparison between yield stress values of paste with FRA
PASTE
CHAPTER 4: Conclusions
This research carried out mortar paste with a volume fraction of fine particles in proportions
of 20, 30, 40 and 45% of its total volume, with w/c ratio and superplasticizer dosage constant, but
the water was adjusted with extra mixing water equivalent to the absorption at 24h of the
aggregates.
Rheological test were able to perform two times on every mixture, on 32’ and 52’ contact,
except for the paste with 45% solid volume fraction of FRA after 15’ mix, due to the fact that it had
a high viscosity. In the case of paste with 20%, 30% solid volume fraction of FNA, very similar
behaviors were observed, while those with FRA were found to have higher differences between the
parties with larger solid volume fractions. In the case of paste with 45% solid volume fraction of
FNA and 40% solid volume fraction of FRA, the self-compacting characteristics were automatically
lost.
The results show that the Modified-Bingham model provides well-defined representation for
mortar paste. The values of yield stress increased with the incorporation of a higher solid volume
fraction of FNA and FRA.
After a longer mixing time in preparation of SCC, the aggregates will generate more fines
particle which can jeopardizes the loss of SCC characteristics. Up to 30% the FRA does not
influence the rheological behavior of paste with less mixing time than 15 minutes.
PASTE
PASTE
[1] Masahiro OUCHI, “Self-Compacting Concrete Development, Applications and

Investigations,” Library (Lond)., no. 2, pp. 2–6.
[2] E. C. Bingham, M. Reiner, S. Sir, and I. Newton, “Rheology,” 2018. .
[3] “ssc.” [Online]. Available: http://www.theconcreteportal.com/scc.html.
[4] “Self-consolidating concrete.” [Online]. Available: https://en.wikipedia.org/wiki/Self-
consolidating_concrete.
[5] S. C. Kou and C. S. Poon, “Properties of self-compacting concrete prepared with coarse and
fine recycled concrete aggregates,” Cem. Concr. Compos., vol. 31, no. 9, pp. 622–627, 2009.
[6] E. Güneyisi, M. Gesoglu, Z. Algin, and H. Yazici, “Rheological and fresh properties of self-
compacting concretes containing coarse and fine recycled concrete aggregates,” Constr.
Build. Mater., vol. 113, pp. 622–630, 2016.
[7] R. J. Flatt et al., “Analysis of superplasticizers used in concrete,” Analusis, vol. 26, no. 2, p.
M 28-M 35, 1998.
[8] L. Evangelista and J. De Brito, “Concrete with fine recycled aggregates: A review,” Eur. J.
Environ. Civ. Eng., vol. 18, no. 2, pp. 129–172, 2014.
[9] D. M. Finkelstein, R. E. Schumacker, and R. G. Lomax, “A Beginner’s Guide to Structural
Equation Modeling,” Technometrics, vol. 47, no. 4, pp. 522–522, 2005.
[10] G. Widmann, “Interpreting TGA curves,” UserCom, pp. 1–20, 2001.

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DISSERTATION THESIS

THE INFLUENCE OF FINE PARTICLES IN

Scientific coordinators: Postgraduate student:

CHAPTER 1: INTRODUCTION AND OBJECTIVES

1.1 Introduction: general concepts

1.2 General objective

CHAPTER 2: STATE OF ThE ART

2.1 Self-compacting concrete

2.2 Recycled aggregates

Figure 1 Cement CEM I 52,5 N-SR 5

The main fields of application are:

Figure 2 Superplasticizer MasterEase 3850

CHAPTER 3: Materials and experimental procedures

3.1 Materials preparations

Figure 3 Drying oven Figure 4 Stored FNA and FRA

3.2 Granulometry determination

Figure 5 5 minutes mixing protocol

Figure 6 15 minutes mixing protocol

Figure 7 Sample splitter Figure 8 The coning and quartering method

Figure 9 Coning and quartering natural sand

Chart 1 Particle size distribution of Recycled Sand

Chart 2 Particle size distribution of Natural Sand

3.3 Mixing procedure

Figure 11 Mortar Paste Mixer Figure 12 Viscometer Viskomat NT

3.4.1 Paste with 0,2 Solid Volume Fraction

Chart 3 Stress grow results-NS, 0,2 Solid Volume Fraction, 0’ mix

Chart 4 Flow curve results-NS, 0,2 Solid Volume Fraction, 0’ mix

Material Weight (g)

Chart 5 Stress grow results-NS, 0,2 solid volume fraction-5’ mix

Chart 6 Flow curve results-NS, 0,2 Solid Volume Fraction, 5’ mix

Material Weight (g)

Chart 7 Stress grow results-NS, 0,2 solid volume fraction-15’ mix

Chart 8 Flow curve results-NS, 0,2 solid volume fraction-15’ mix

Material Weight (g)

Chart 9 Stress grow results-RS, 0,2 solid volume fraction-0’ mix

Chart 10 Flow curve results-RS, 0,2 solid volume fraction-0’ mix

Material Weight (g)

Chart 11 Stress grow results-RS, 0,2 solid volume fraction-5’ mix

Chart 12 Flow curve results-RS, 0,2 solid volume fraction-5’ mix

Material Weight (g)

Chart 13 Stress grow results-RS, 0,2 solid volume fraction-15’ mix

Chart 14 Flow curve results-RS, 0,2 solid volume fraction-15’ mix

3.4.2 Paste with 0,3 Solid Volume Fraction

Material Weight (g)

Chart 16 Flow curve results-NS, 0,3 solid volume fraction-0’ mix

Material Weight (g)

Chart 17 Stress grow results-NS, 0,3 solid volume fraction-5’ mix

Chart 18 Flow curve results-NS, 0,3 solid volume fraction-5’ mix

Material Weight (g)

Chart 19 Stress grow results-NS, 0,3 solid volume fraction-15’ mix

Chart 20 Flow curve results-NS, 0,3 solid volume fraction-15’ mix

Material Weight (g)

Chart 21 Stress grow results-RS, 0,3 solid volume fraction-0’ mix

Material Weight (g)

Chart 24 Stress grow results-RS, 0,3 solid volume fraction-5’ mix

Chart 25 Flow curve results-RS, 0,3 solid volume fraction-5’ mix

Material Weight (g)

Chart 26 Stress grow results-RS, 0,3 solid volume fraction-15’ mix

Chart 27 Flow curve results-RS, 0,3 solid volume fraction-15’ mix

3.4.3 Paste with 0,4 solid volume fraction

Material Weight (g)

Chart 28 Stress grow results-RS, 0,4 solid volume fraction-0’ mix

Chart 29 Flow curve results-RS, 0,4 solid volume fraction-0’ mix