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A comprehensive approach for designing workable bio-based cementitious

composites

M’hamed Yassin Rajiv da Gloria, Vanessa Maria Andreola, Daniele Oliveira Justo dos
Santos, Marco Pepe, Romildo Dias Toledo Filho
PII: S2352-7102(20)32022-2
DOI: https://doi.org/10.1016/j.jobe.2020.101696
Reference: JOBE 101696

To appear in: Journal of Building Engineering

Received Date: 20 May 2020

Revised Date: 18 July 2020
Accepted Date: 22 July 2020

Please cite this article as: M’.Yassin.Rajiv. da Gloria, V.M. Andreola, D.O.J. dos Santos, M. Pepe, R.D.
Toledo Filho, A comprehensive approach for designing workable bio-based cementitious composites,
Journal of Building Engineering (2020), doi: https://doi.org/10.1016/j.jobe.2020.101696.

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 Credit Author Statement

M’hamed Yassin Rajiv da Gloria:

Methodology, Data Curation, Investigation, Formal analysis, Writing - Original Draft

Vanessa Maria Andreola

Methodology, Data Curation, Investigation, Formal analysis, Writing - Original Draft

Daniele Oliveira Justo dos Santos

Methodology, Data Curation, Investigation, Formal analysis, Writing - Original Draft

Marco Pepe:
Conceptualization, Data Curation, Formal analysis, Writing - Original Draft, Writing - Review &
Editing, Supervision

Romildo Dias Toledo Filho:

Conceptualization, Writing - Review & Editing, Supervision, Project administration
 A COMPREHENSIVE APPROACH FOR DESIGNING WORKABLE

BIO-BASED CEMENTITIOUS COMPOSITES

M’hamed Yassin Rajiv da Gloria

Department of Civil Engineering, Federal University of Rio de Janeiro COPPE/UFRJ
P.B. 68506, CEP 21941-972, Rio de Janeiro-RJ, Brazil.
e-mail: ydagloria@yahoo.fr

Vanessa Maria Andreola

Department of Civil Engineering, Federal University of Rio de Janeiro COPPE/UFRJ
P.B. 68506, CEP 21941-972, Rio de Janeiro-RJ, Brazil.
e-mail: vanessa.andreola@coc.ufrj.br

Daniele Oliveira Justo dos Santos

Department of Civil Engineering, Federal University of Rio de Janeiro COPPE/UFRJ
P.B. 68506, CEP 21941-972, Rio de Janeiro-RJ, Brazil.
e-mail: danielejusto@gmail.com

Marco Pepe
Department of Civil Engineering, University of Salerno, Italy
TESIS srl, Fisciano (SA), Italy
e-mail: mapepe@unisa.it
m.pepe@tesis-srl.eu

Romildo Dias Toledo Filho

Department of Civil Engineering, Federal University of Rio de Janeiro COPPE/UFRJ
P.B. 68506, CEP 21941-972, Rio de Janeiro-RJ, Brazil.
e-mail: toledo@coc.ufrj.br

Corresponding author: toledo@coc.ufrj.br

1
ABSTRACT

The present work proposes a generalized method for designing moldable bio-concretes,

incorporating three types of vegetable residues (wood shaving, bamboo particles and rice husk)

which are employed as bio-aggregates within a cement-based matrix.

The above-mentioned procedure is based, first of all, on a fundamental physical and

morphological characterization of the bio-aggregates as well as on the analysis of their

compatibility with cement-based matrices. Then, considering the specific features of the employed

bio-aggregates, a novel approach is also presented for the mixing production process of bio-

concretes mixtures with the aim of warranty an adequate consistency and easy moldability at the

fresh state. Finally, a comprehensive experimental campaign is performed with the aim of analyzing

the influence of bio-aggregates on the bio-concretes performances at hardened state.

The analysis proposed herein unveils the existing relationship between compressive strength,

water-to-cement ratio, cement consumption and bio-concrete density leading to a proposed

simplified design abaci. Considering the rational nature of the proposed approach, it can be easily

extended to others kind of bio-aggregates that could be considered for producing workable bio-

concretes.

2
KEYWORDS: Mix-design, Bio-based cementitious composites, Bio-aggregates, Wood-Bio-

concrete, Bamboo-Bio-concrete, Rice Husk- Bio-concrete, Workability, Mechanical properties.

3
1. INTRODUCTION

Nowadays, enhancing the environmental sustainability is a worldwide common challenge in various

sectors of modern research and technology also for industrial processes [1] and, the “greening” of

the concrete industry also represents one of the main goals for policy makers and private

companies, as well as for the scientific community [2]-[3].

In view of this, the scientific community is getting more and more interested in exploring the

potential of bio-based cementitious composites in construction obtained by including some non-

conventional constituents in mortars and concrete [4]-[6], derived from either processing parts of

plants (either leaves or stems) or recycling waste produced in agriculture [7]-[8].The lignocellulosic

materials are, generally, available in large quantities and, in addition, the specific properties of the

aforementioned bio-based constituents (such as, lightweight, high porosity and water absorption

capability, low thermal conductivity, etc.) can lead to composite materials characterized by an

enhanced performance with regards to either the mechanical or the physical-thermal behavior [9]-

[11].

More specifically, in the last decade researchers have been focusing on experimental and

theoretical studies aimed at analyzing the physical and mechanical behavior of composite systems

incorporating vegetal fibers/textile employed as spread [12]-[15] and/or continuous [16]-[18]

reinforcement and mortars and concretes incorporating bio-aggregates for the partial-to-total

replacement of ordinary aggregates leading to the so-called bio-concretes [19]-[20].

According to several experimental evidences available in the literature, one of the main issues

related to the use of bio-aggregates in mortar and/or concrete is their compatibility with the cement-

based matrix. For this reason, before being employed as alternative aggregates, the bio-particles

require some type of treatment which allows to reduce/remove inorganic substances and water-

soluble extractives for enhancing their durability when embedded within a cementitious matrix

4
while at the same time mitigating the possible retardation/inhibition of the cement hydration [21]-

[24].

Another fundamental issue is related to the production method for bio-based composites.

Since the bio-aggregates are characterized by a significant water absorption capacity and low

density, in comparison with conventional concrete constituents, their presence within the cement-

based batches limits the use of traditional mixing procedures. If not properly controlled, the

presence of porous and lightweight bio-particles affects the fresh mixture properties such as

moldability, segregation and exudation, besides their hardening properties, due to a potential

retardation and strength development. In the current practice, a bio-concrete is produced using

mechanical compactions which requires the use of specific machineries. This technique limits the

feasibility of producing bio-concretes using the traditional concrete practices that are well

disseminated around the world. It is worth mentioning that when the bio-aggregates are subjected to

compaction actions, the porous aggregates may be significantly deformed, losing their original

micro-structure and partially reducing the lightweight characteristics of the resulting bio-concretes

[25]-[26]. In order to have more workable mixtures, it has been proposed [27]-[28] to pre-saturate

the vegetable particles for not affecting the effective water within the mixture controlling both the

fresh workability and hardened properties of the bio-concrete. This approach may present practical

limitations for applications on a large scale. For the above-mentioned reasons, further research is

required for improving and simplifying the processing procedures for bio-concretes.

In addition, the mix-design methods for bio-concrete still follow empirical rules in their

methodological approach. Consequently, the definition of reliable relationships capable of

predicting and controlling the relevant properties of bio-concrete mixtures is still an open issue in

this research area. As normally occurs, when novel “ingredients” are considered within the design

of innovative cementitious matrices [29]-[31], specific mix-design methods are required for their

diffusion at large scale.

5
 In this context, the present study, being based on a fundamental physical-chemical and

morphological characterization of three types of vegetable residues (employed as bio-aggregates),

proposes an adaption of traditional mix-design and mixing processes for the development of

moldable bio-concrete mixtures. The proposed methods are based on a comprehensive experimental

campaign aimed at analyzing the influence of bio-aggregates types and amount on the key physical

and mechanical performance on the resulting cement-based bio-composites at both fresh and

hardened state. By following the approach proposed in the present study, the traditional concrete

industry can use their current line of production for implementing the bio-concrete mixtures. Since

the results presented herein are based on testing three morphologically and microstructurally

different types of bio-aggregates, the proposed methods can be easily extended to other kind of bio-

concretes.

6
2. MATERIALS AND METHODS

2.1 Cement and admixtures

A high initial strength Portland cement (density equal to 3170 kg/m3) produced by Holcim, and

labelled CP V-ARI in accordance with the National Brazilian Standard [32] was utilized for the bio-

concretes production. The chemical composition of the employed cement is summarized in Table 1.

The adoption of this type of binder is mainly related to its high initial resistance that is,

generally, adequate for prefabricated elements. Despite this choice not being the most “sustainable”

one, it is worth highlighting that the key goal of the present study is to investigate the influence of

bio-aggregates on the resulting performance of Portland cement-based composites at both fresh and

hardened states. As will be mentioned in the conclusions, in further studies, the possible

employment of supplementary cementitious materials will be also investigated.

A Viscosity Modifying Agent (VMA), manufactured by BASF (MasterMatrix UW 410) [33]

and characterized by a density of 0.7 g/cm³, was used with the purpose of providing the required

consistence at the fresh state. In addition, Calcium Chloride (CaCl2) was incorporated as setting

accelerator in the wood bio-concretes.

2.2 Bio-aggregates

2.2.1 Physical and morphological properties of bio-aggregates

Three types of vegetable residues were employed in this study as bio-aggregates: wood shavings

(WS), bamboo particles (BP) and rice husk (RH).

The WS bio-aggregates were derived from residues of woodworking activities of carpentry of

specie Pinus elliottii Engelm. In order to reduce the average water absorption of this bio-source, the

shavings characterized by a nominal diameter lower than 1.18 mm were removed due to their

greater specific area. The BP bio-aggregates were obtained by processing the waste of the culms

derived from cuttings of Dendrocalamus Asper bamboo, available in the region of Rio Grande do

7
Sul (BR). Specifically, the waste culms, characterized by an average length of 45 cm, were reduced

to particles (maximum nominal diameter of 4.75 mm) by using both an industrial crusher and a

knife mill. Finally, the RH were derived from rural producers located in the São Paulo (BR) region.

This type of bio-aggregate is characterized by a narrow length distribution ranging from 5 mm to 8

mm and a maximum width of 4 mm.

An overview of the bio-aggregates employed in this study is given in Figure 1.

In order to characterize the bio-aggregates, their bulk specific density, apparent density [34]

and moisture content [35] were determined. The water absorption capacity of the bio-aggregates

was estimated by also taking into account the mixing time for the bio-concretes production (as

described in section 2.3.1). Specifically, for both WS and BP, a representative sample of bio-

aggregates (100 g) were mixed in half a liter of water for 8 min (estimated bio-concrete mixing

time); after mixing, the aggregates were passed through a 150 μm sieve to drain the excessive water

and air-dried until reaching the saturated surface dry (SSD) condition of the bio-aggregates sample.

Then, the bio-aggregates were weighed and the water absorption determined. For RH bio-

aggregates, the time evolution of the water absorption was estimated by using measurements

recently proposed in the literature [26]. The results summarizing the physical properties of the bio-

aggregates are reported in Table 2.

In addition, a fundamental morphological characterization of the employed bio-aggregates

was performed by using an Aggregate IMaging System (AIMS) which furnishes shape 2D and

angularity indices of the particles [36]. Specifically, the shape 2D index relates to the shape of a

circle and ranges from 0 (for circular particles) to 20 while the angularity index, describing the

variations in the contour of the analyzed particles, ranges from 1 (perfect circle) to 10000. The

results of this analysis are summarized in the last columns of Table 2. In accordance with the

classifications reported in the literature [36], all the employed bio-aggregates can be classified as

“elongated” in relation to the shape 2D index but based on the angularity index both WS and BP

bio-aggregates are classified as “sub-angular”, while the RH can be classified as “sub-rounded”.

8
2.2.2 Bio-aggregates compatibility with cement paste

As already well known from the literature, the extractives present in the vegetable bio-aggregates

are the main responsible for the inhibition/retardation of the setting and hardening phases of cement

hydration [23]- [25].

In order to mitigate this phenomenon, as already proposed in previous works [37], and in

order to remove the water-soluble extractives, the bio-aggregates were washed in hot water at 80° C

for 1 hour, considering a bio-aggregates-to-water mass proportion equal to 1:10. The washing

procedure was repeated for five cycles and, after each washing cycle, the extractive content in the

water was determined. The water of each cycle was passed through a 150 μm sieving mesh. From

the wastewater, samples were placed in a temperature-controlled room (i.e., 40° C) for 36 hours

which was the time necessary to eliminate the water by evaporation, leaving only the extractives.

After the multiple washings in hot deionized water and after drying off waste waters, a

gradual variation of the water coloration was observed as shown in Figure 2 where, starting from

the left to the right, the first wastewater was dark, and the following got clearer after further

washings. The change of the color shade can be explained by the fact that the washing cycles

removed a significant amount of water-soluble extractives (for instance, the extractives responsible

of color). This evidence is confirmed by the data plotted in Figure 3 where it is possible to identify

the progressive reduction of extractive concentrations for the bio-aggregates after the several

washing cycles.

A more fundamental approach is also presented for evaluating the efficiency of the bio-

aggregates washing cycles by performing isothermal calorimetry tests on cement pastes produced

with the wastewaters derived from the washing process (Figure 2). The tests were performed at a

temperature of 27 °C for a period of 7 days. Specifically, these tests were aimed at evaluating the

influence of the extractive amount on the cement hydration kinetics. A reference cement paste

(water-to-cement ratio equal to 0.45) was produced with deionized water while additional cement

pastes were prepared with wastewater derived from the washing cycles of the bio-aggregates.

9
Figure 4 shows the resulting heat-flow curves obtained from the isothermal calorimetry tests

obtained for the cement paste produced with wastewater derived from the BP bio-aggregates

washings. The curves confirm that the presence of extractives affects the cement hydration (mainly

for the induction period). A more relevant hydration delay is observed for the cement paste

containing the wastewater after 1 washing cycle. For instance, the induction period was completed

in 1.3 hours for the Reference paste, while the Wastewater 1 cycle paste showed a delay of around

3.0 hours. It is worth mentioning that already with the wastewater of cycle 2 the hydration is

significantly improved, having an almost negligible influence when wastewater 4 is used. Similar

results were obtained also for the cement pastes produced with wastewater derived from the

washing cycles of rice husk bio-aggregates.

The data presented in both Figure 3 and Figure 4 demonstrate that the reduction of

extractives is more significant during the first cycles. For instance, more than 80 % of reduction is

registered for bamboo particles and rice husk after the first washing cycle, while a similar reduction

was obtained for wood shaving bio-aggregates after three washing cycles.

For these reasons, additional calorimetry tests were performed in order to discover the influence

of 1 and 3 WS washings on the cement hydration. The approach used was based on comparing the kinetics

of the reference cement paste and cement pastes mixed with fine WS bio-aggregates washed 1 and 3 times

(WS-1 cycle and WS-3 cycles). Fine grained WS were used to allow the mixture preparation for the

calorimeter ampoule. The deionized water-to-cement and the fine WS-to-cement ratios were 0.45 and 0.075,

respectively. The mixtures preparation consisted of hand-mixing the cement and deionized water during 1

min in a glass beaker, followed by adding the dry fine WS and a further mixing for 1 min.

According to Figure 5, the mixture WS-1 cycle presented a complete hydration inhibition while WS-3

cycles showed a hydration delay with a lower heat flow when compared with the reference. The mixture WS-

1 cycle stayed in induction stage until the end of the test; therefore, the acceleration did not happen. The

explanation of this fact is that the extractives present in the unwashed WS inhibited the cement hydration, as

the quantity of extractives removed after only one washing cycle was not enough to allow the cement setting.

10
Concerning the WS-3 cycles, an acceleration period was clearly observed although its profile showed a

hump, probably due to the delay of cement hydration products.

In accordance with these evidences and in order to optimize the processing procedures, the

wood shavings were washed three times and it was necessary to add CaCl2 to accelerate the cement

hydration. Both the bamboo particles and rice husks were subjected to only one cycle of washing

before being employed as bio-aggregates for the production of bio-concretes, without any addition

of accelerators.

2.3 Bio-concrete

The bio-concrete mixtures were produced by considering the variation of the following parameters:

(i) type of bio-aggregates (i.e., wood shavings, bamboo particles and rice husks); (ii) volumetric

fraction of the bio-aggregates (i.e., 45%, 50% and 52.5%) and; (iii) water-to-cement ratios (i.e.

0.40, 0.45 and 0.50).

As also mentioned in the introduction section, the key goal of this study was to produce bio-

concretes presenting a adequate workability of the mixtures at the fresh state. Specifically, all the

mixtures were prepared for obtaining a consistence index of around 275±30 mm that, generally, is

indicative of a good moldability.

One of the key aspects of the mixture proportioning for bio-concretes is related to the water

that is absorbed by the bio-aggregates during the mixing processes. Since vegetable bio-aggregates

are characterized by high values of water absorption (e.g., higher than 100 %) both concrete

workability and cement setting, as well as hardening processes can be strongly influenced by the

methodology adopted for saturating the bio-aggregates employed within the cement-based paste.

For instance, researchers demonstrated that in wood-cement composite mixtures the water amount

should be sufficient for keeping the particles saturated in order to allow the cement hydration and

also to guarantee the consistence of the mixture [38]. Moreover, it is worth mentioning that one of

the objectives of this study is to propose a bio-concrete processing procedure in which the bio-

aggregates are employed at dried state. In fact, in the view of a possible scaling up of the procedures

11
proposed herein, the employment of particles without a pre-saturation stage would facilitate the bio-

concrete production at industrial scale.

To reach the target workability and spreading, 3 mixing sequences were tested on the bio-

concrete mixtures presenting a cement-to-bio-aggregates ratio equal to 2.5 and water-to-cement

ratio equal to 0.45. The first attempt consisted of a pre-mixture of cement and dry bio-aggregates (2

min), followed by a progressive addition of water during 5 min. In the second approach, the cement

paste was produced first and the bio-aggregates gradually added. The third sequence consisted of a

mixture of bio-aggregates and water, followed by the cement addition. According to the spreading

test performed, the consistence indexes presented after the first, second and third mix methods were

260 mm, 200 mm and 170 mm, respectively. It is worth mentioning that a high exudation and

segregation was observed when using the second approach. The first method presented only a slight

paste exudation and a spreading index close to the target of the current study. To reduce the

exudation and guarantee the cohesion of the bio-concrete produced using the first procedure, small

proportions of VMA were used in the mixture leading to the desired workability and consistence

without phase segregation. Consequently, in the present study, all the bio-aggregates were

employed at dried state and the total water amount considered for the mixture production was

determined considering the sum of the water for cement hydration (i.e., effective water) and an

additional amount of water (i.e., compensating water) based on the absorption capacity of the bio-

aggregate presented in Table 2.

The mixing procedure consisted in homogenizing the raw materials (cement and dry bio-

aggregates) with subsequent addition of water. The amount of VMA used was 0.13% and the target

spreading for all mixtures was 275 ± 15 mm. With this approach, a bioconcrete with a good

homogeneity and moldability was produced. As already mentioned, calcium chloride (CaCl2) was

used for the wood shaving composites as setting accelerator.

The mixture proportioning of the bio-concretes were calculated as shown in Table 3. The

labels for the Wood Bio-Concrete (WBC), Bamboo Bio-Concrete (BBC) and Rice husk Bio-

12
Concrete (RBC) mixtures represent the variation of the bio-aggregates volumetric fractions (i.e.,

45%, 52% 52.5% ) and the water-to-cement ratio (i.e., 0.40; 0.45 and 0.50).

2.3.1 Samples fabrication and experimental tests

The bio-concretes mixtures were produced by adopting the following procedure: after a hand mix of

the dry bio-aggregates and cement, the mixture was introduced into a 5 l mixer at low speed (136

rpm). During the first 2 minutes, the water was slowly added, followed by the addition of the VMA

at the 5th minute. The mixing continued until it reached 8 minutes of total time.

At the fresh state, the consistence index was measured by performing flow table tests in

accordance with National Brazilian Standard [39].

The fresh bio-concretes were molded in cylindrical molds (d=5cm and h=10 cm) in three

layers. Each layer was mechanically vibrated on a vibratory table (68 Hz) during 10 seconds. The

bio-concretes were kept in the molds up to 24 hours. The bio-concretes were cured in a vapor

chamber at 20 ± 2°C and 95 ±2% RH up to the testing age. To measure the densities, 4 samples of

the bio-concretes were dried during one week at 60 °C until a constant mass was reached. Then, the

samples were weighed to the nearest 0.01g and the dimensions measured with a paquimeter.

For each curing age (i.e., 7 and 28 days), compressive strength tests were performed on four

samples by using the universal testing machine Shimadzu-1000 kN, at the rate of 0.3 mm/min. The

compressive strength and the elastic modulus were determined according to the National Brazilian

Standard [40].

13
3. EXPERIMENTAL RESULTS

Table 4 presents an overview of the experimental results obtained in the present research.

3.1 Workability

Figure 6 shows the consistence at fresh state obtained for representative bio-concretes samples

produced in this study. The BBCs and RBCs presented a similar consistence at the fresh state, while

the WBC showed the highest values. The data reported in Table 4 confirm that, by adopting the

proposed mixing processing procedure, the desired consistence (i.e., spreading ranging between 260

mm and 290 mm) was always achieved.

Moreover, it is worth mentioning that, the use of a fixed percentage of VMA (in relation to

the cement amount) warranties the homogeneity and the fluidity of the mixture. The data highlight

that, as a general trend, the bio-concrete workability increases for higher amount of effective water

as well as for higher values of cement content (see Table 3 and Table 4).

Finally, all mixtures show adequate workability for molding with biomorphic format. This

makes the mixing method versatile, considering that without applying any type of pressure it is

possible to fill a desired shape.

3.2 Density

The densities (at the hardened state) of bio-concretes range between 820 - 960 kg/m3, 615 - 800

kg/m3 and, 640 - 900 kg/m3 for WBC, BBC and RBC mixtures, respectively (Table 4). It can be

noted that the density (γ) at the hardened state of the produced cement-based composites is directly

related to the cement and water amount present in each mixture. It decreases for higher values of

water-to-cement ratio and increases for the mixtures containing an higher amount of cement.

Specifically, the bio-concretes with bio-aggregates volume of 52.5% and a water-to-cement ratio of

0.50 presented the lowest density, which can be justified due to the higher volume of particles and

the greater volume of total water in the mixture, causing voids to appear in the hardened material.

14
Although the RH are lighter than BP, the BBC showed lowest density, which can be attributed to

the internal porosity create within the BBC. It is worth mentioning that, all the produced bio-

concretes can be classified as lightweight concretes, for presenting densities lower than 1800 kg/m³

[41]. Considering these classificatory limits, all mixtures of RBC and BBC showed densities up to

three times less. Although the WBC 45-0.40 mixture is the most dense, it still presents 88% less

density than the one proposed for light concrete.

According to the results exposed in Table 4, WBC presented the highest densities. This can

be justified by the lowest compensating water used to produce the WBC mixtures. In fact, WBC

was manufactured by compensating water 17% and 24% lower than that of BBC and RBC,

respectively. At hardened state, WBC 52.5 presented an average of densities 24% and 20% higher

than that of BBC and RBC, respectively. The same trend was observed with WBC 50 and WBC 45.

Previous studies in the literature reported that the densities of bio-concretes were higher than

those achieved in the present research. This is due to the method typically applied for molding the

bio-concrete samples (i.e., mechanical compaction) that compresses the particles during the filling

of the molds. Andreola et al. [37] in the production of bamboo bio-concretes using manual pressing,

obtained densities of 1070 and 1100 kg/m³ for BBC 50-0.40 and BBC 45-0.40, respectively. Da

Gloria et al. [38], adopting manual compaction in the production of wood bio-concrete (WBC),

obtained density of 1100 and 1200 kg/m³ for the WBC 50-0.40 and 45-0.40, respectively. This

result highlights the fact that the proposed methodology and mix design leads to have reduced

density with a consequent improvement of the thermal efficiency of the resulting hardened bio-

concrete elements/products.

3.3 Mechanical properties

Before analyzing the results in term of mechanical properties, it is worth highlighting that the

produced bio-concretes present a high homogeneity at the hardened state. Based on the

representative image shown in Figure 7 a homogeneous distribution of the bio-aggregates along the

15
entire length of the samples is evident, without the presence of segregation in any part of the bio-

concretes, which proves the uniformity of the mixtures analyzed herein. This evidence is also

confirmed by the low standard deviation (s.d.) registered for each type of test (see Table 4).

The compressive strength of the bio-concretes (obtained at both 7 and 28 days of curing) and

the Elastic modulus at 28 days are summarized in Table 4, while representative stress-strain curves

are reported in Figure 8, Figure 9 and Figure 10 for WBC, BBC and RBC mixtures, respectively.

The stress strain curves showed an initial elastic linear behavior followed by a non linearity,

until reaching the maximum compressive strength followed by a non linear descending branch

which is more pronunced for the bio-concrete characterized by the highest water-to-cement ratios

(Figure 8, Figure 9 and Figure 10).

The linear behaviour of WBC 52.5, WBC 50 and WBC 45 curves was observed until 50%,

47% and 44% of the strength peak value. From the peak strain and up to the strain of 8000 µɛ, all

WBC registered an average load decay of 15%. It illustrated the energy absorption capacity

provided to the mixtures by the high agregates volumes. After 7 curing days, all the mixtures

reached more than 70% of the strength registered at 28 days,which confirms the efficency of the

combined effect of using a cement with high initial resistance and the washing treatments on the

potential delay of the cement hydration processes due to the presence of extractive within the bio-

aggregates. At 28 days, the cylindrical compressive strengths ranged from 3.60 to 8.90 MPa for

WBC, from 2.50 to 4.60 MPa for BCC and from 1.30 to 3.60 MPa for RBC mixtures. (see Table

4). Specifically, the Bio-concrete 52.5-0.50 mixtures always presented the lowest value for each

type of employed bio-aggregates. This can be justified by the fact that this mixture included the

highest volume of both bio-aggregate and water amount within the mixtures (Table 3). Although

the bio-concrete 45-0.40 mixtures showed the highest resistance, they are characterized by the

lowest volume of bio-aggregates and the lowest amount of water.

When considering on one hand WBC of same water-to-cement ratio, it can be observed that

the decrease of 2.5% of bio-aggregates from WBC 52.5 to WBC 50 lead to a strength increase of

16
33%, while a strength increase of 28% was registered from WBC 50 to WBC 45. On the other hand,

an increase of 0.05 of water-to-cement ratio from 0.4 to 0.45 of WBC containing the same

volumetric fraction lead to an average strength decrease of 17%, while a lower decrease of 10% was

observed from 0.45 to 0.50.

At 28 days, BBC 52.5-0.4 to 0.50 showed an increase in resistance of 30%, while BBC 45-0.4

to 0.5 increased by 19%. From BBC 52.5 to 45 there was an increase in resistance of 38% (w/c 0.4)

and 51% (w/c 0.4). Comparing the strength at 28 days, the WBC presented the highest compressive

strength, while the BBC and the RBC were respectively 48% and 60% lower for mixing bio-

concretes with a bio-aggregates volume of 45% and a water-to-cement ratio of 0.4. The low

resistance showed by the RBC mix may be attributed to its high water content.The values achieved

in terms of compressive strength at 28 days are lower than the results found in the literature. This is

also related to the fact that, in the literature, generally, a cold pressing or compaction is adopted for

the bio-concrete production, since the mixture does not present an adequate workability at the fresh

state. With mechanical pressing, the height that fills the mold is compacted and eliminates voids,

resulting in a bioconcrete with greater resistance, but a much higher density.

Finally, Figure 11 reports the relationship between the elastic modulus and the corresponding

compressive strength: it is worth mentioning that the general trend is independent of the type of bio-

aggregates employed within the cementitious matrix. Moreover, in Figure 11 a possible

relationship between the bio-concrete compressive strength and the corresponding elastic modulus

is proposed also based on the same correlation defined by the fib Model Code [43] for structural

concrete:

β
f 
E = α⋅  c  (1)
 10 

where E is the elastic modulus of concrete in MPa, fc is the compressive strength in MPa and α

(equal to 3.60) and β (equal to 0.60) are two coefficient that were calibrated based on the

experimental data obtained in the present study. It is worth highlighting that the proposed

17
calibration is valid for bio-concrete mixtures in which the cement-to-bio-aggregates ratio fits within

the range explored herein and, moreover, it is valid only when Portland cements with a high amount

of clinker (i.e., above 90%) are employed.

18
4. RATIONAL DOSAGE METHOD FOR BIO-CONCRETE

The results presented herein allowed a comprehensive analysis leading to propose a rational

approach for the mixture proportiong of bio-concrete mixture of adequate workability for

moldability and desired strength/density. The proposed design method allows the production of bio-

concretes without deforming or crushing the bio-aggregates, taking advantage of keeping the

peculiar characteristic of these bio materials (i.e., lightweight).

Specifically, moving from the results achieved herein, a mix-design diagram is presented in

Figure 12 (for WBC) Figure 13 (for BBC) and Figure 14 (for RBC) by correlating cylindrical

compressive strength at 28 days, water-to-cement ratio, bio-concrete density and cement

consumption.

The analytical expression correlating the compressive strength and the effective water-to-

cement ratio is based on the well know Abram’s law:

k1
fcm,28days = w (2)
( k2 ) c

where k1 and k2 are two constant values calibrated for each class of bio-concrete that include the

same amount of bio-aggregates (i.e., bio-concrete 45%, 50% and 52.5% ) and types of bio-

aggregates (i.e., wood shavings, bamboo particles and rice husk), and the compressie strength is

expressed in MPa.

Then, a direct correlation is proposed between density and compressive strength:

f cm,28days = k 3 ⋅ γ 3 (3)

where k3 is a constant value, the compressive strength are expressed in MPa and the density in

g/cm3.

Finally, a linear relationship is proposed between the water-to-cement ratio and the cement

consumption (in kg/m3):

19
 w
cem = k 4 − k 5 ⋅ (4)
c

where k4 and k5 are two constant values calibrated for each class of bio-concrete that include the

same amount of bio-aggregates (i.e., bio-concrete 45%, 50% and 52.5% ).

The values calibrated for the five constant values for each group of bio-concrete mixtures are

summarized in Table 5.

The proposed diagram (see Figure 12, Figure 13 and Figure 14) can represent an useful tool

for designing and producing workable bio-concretes. For instance, once the density and/or

compressive strength are defined, it is possible to obtain the bio-aggregate volume, the water-to-

cement ratio as well as the cement consumption by warranting an adequate moldability and

workability at the fresh state (i.e., spreading value in the range of 260 to 290 mm). This, certainly,

represents a fundamental tool for upscaling the development of bio-based construction materials

since this approach can be easily extended to other types of vegetable residues, able to be

implemented as raw aggregates for cement-based mixture production. Considering the lack of

analytical tools available in the literature for the bio-concrete mix design, the proposed approach

could promote the development of new alternative sustainable construction materials.

A further step would be the possibility to investigate the feasibility of the combined use of

alternative binders and bio-aggregates with the two-fold objective of both reducing the Portland

cement amount and increase the bio-concrete durability.

Finally, it is worth highlighting that the peculiar characteristics of the bio-concretes could find

several possible applications in the construction sector. For instance, one of the most promising

solutions could be the implementation of sandwich panels composed by outer structural concrete

layers and a thermally efficient lightweight core made of bio-concrete. This leads to having pre-cast

lightweight panels that can be efficiently used for both new building construction as well as for the

thermal and structural retrofitting of the existing ones.

20
5. CONCLUSIONS

This work presents the results of a comprehensive experimental study on bio-based cementitious

composites incorporating wood shavings, bamboo particles and rice husk as bio-aggregates.

In accordance with the results obtained herein, the following conclusions can be drawn:

• The preliminary washing treatments on bio-aggregates proved to be essential for removing

the water-soluble extractives and improving the compatibility between Portland cement and

vegetable residues employed within the cementitious matrix;

• The accurate test, proposed herein for evaluating the water absorption capacity during the

mixing process, was fundamental for ensuring the desired controlled workability of the bio-

concretes at the fresh state;

• The achievement of a mixing production method in which the bio-aggregates are employed

at the dry state and, at the same time, no compaction is required for molding the samples,

represents a significant improvement for the possible upscaling of bio-based composites;

• The good workability of the bio-concretes warrants an homogeneous distribution of the bio-

aggregates along the entire length of the samples: this also leads to a significant low scatter

of the experimental results;

• The proposed design diagrams represent a useful tool for designing and producing workable

bio-concretes. This, certainly, represents a fundamental step for upscaling the development

of bio-based construction materials since this approach can be easily extended to other types

of vegetable residues for being employed in cement-based composites.

21
6. ACKNOWLEDGEMENTS

Authors and scholarship holders would like to express their gratitude to Conselho Nacional de
Desenvolvimento Científico e Tecnológico – Brasil – (CNPq). This study was financed in part by
the Coordenação de Aperfeiçoamento de Pessoal de Nível Superior- Brasil (CAPES) - Finance
Code 001.
The present study is also part of the activities carried out by the authors within the
“SUPERCONCRETE” Project (www.superconcrete-h2020.unisa.it) funded by the European
Union's Horizon 2020 Research and Innovation Programme under Grant Agreement No 645704
(H2020-MSCA-RISE-2014).

22
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26
 (a) (b) (c)

Figure 1. Bio-aggregates employed in this study: (a) Wood Shaving-WS, (b) Bamboo Particles – BP, (c) Rice Husk - RH.

27
 Wastewater 1 Wastewater 2 Wastewater 3 Wastewater 4 Wastewater 5
Wood Shaving
Bamboo Particles
Rice Husk

Figure 2. Wastewater for bio-aggregates after several washing cycles.

28
 0.30

Extratives amount [%]

Wood Shavings
Bamboo Particles
Rice Husk

0.20

0.10

0.00
1 2 3 4 5
Washing cycles

Figure 3. Progressive reduction of extractive concentrations.

29
 8

Heat flow [mW/g]

Reference
7 Wastewater 1 cycle
Wastewater 2 cycles
Wastewater 4 cycles
6

0
0 3 6 9 12 15 18 21 24
Time [h]

Figure 4. Hydration kinetics for cement pastes produced with bamboo particles wastewater.

30
 8

Heat flow [mW/g]

Reference
7
WS - 1 cycle

6 WS - 3 cycles

0
0 12 24 36 48 60 72
Time [h]

Figure 5. Hydration kinetics for cement pastes produced with washed WS bio-aggregates.

31
285 mm 270 mm 274 mm

(a) WBC (b) BBC (c) RBC

Figure 6. Representative spreading and consistence index for bio-concrete mixtures.

32
Figure 7. Representative homogeneous samples of hardened wood bio-concretes mixture.

33
Figure 8. Stress-strain curves for Wood Bio-Concretes after 28 days of curing.

34
Figure 9. Stress-strain curves for Bamboo Bio-Concretes after 28 days of curing.

35
Figure 10. Stress-strain curves for Rice-Husk Bio-Concretes after 28 days of curing.

36
 4

Elastic Modulus [GPa]

3

1
WBC
BBC
RBC
0
0 2 4 6 8 10
Compressive strength [MPa]

Figure 11. Compressive strength vs Elastic Modulus for bio-concrete mixtures.

37
Figure 12. Rational mix-design diagram for Wood Bio-Concrete (WBC) mixtures.

38
Figure 13. Rational mix-design diagram for Bamboo Bio-Concrete (BBC) mixtures.

39
Figure 14. Rational mix-design diagram for Rice husk Bio-Concrete (RBC) mixtures.

40
Table 1. Chemical properties of cement.
Chemical composition (%)
CaO 68.973
SiO2 14.955
Al O 4.700
2 3
Fe2O3 3.500
SO3 4.290
K2O 0.980
SrO 0.420
TiO2 0.140
MnO 0.014

41
Table 2. Physical properties for bio-aggregates.
Density Apparent density Moisture content Water absorption AIMS
Bio-aggregates
(kg/m3) (kg/m3) (%) (%) Shape Angularity
Wood shavings 1250 550 14 100 13.68 4521
Bamboo particles 1430 580 11 110 14.91 4152
Rice husk 1020 300 12 228 15.20 3172

42
Table 3. Bio-concrete mixture composition.
Cement Bio-aggregates Effective water Compensating water VMA CaCl2
Bio-aggregate type Mixture w/c
(kg/m3) (kg/m3) (kg/m3) (kg/m3) (kg/m3) (kg/m3)
WBC 52.5-0.40 0.40 674 284 269 284 1.35 20.25
WBC 52.5-0.45 0.45 652 284 293 284 1.31 19.59
WBC 52.5-0.50 0.50 632 284 316 284 1.26 18.97
WBC 50-0.40 0.40 711 275 284 275 1.42 21.35
Wood WBC 50-0.45 0.45 687 275 309 275 1.37 20.62
WBC 50-0.50 0.50 664 275 332 275 1.33 19.93
WBC 45-0.40 0.40 775 247 258 247 3.10 23.25
WBC 45-0.45 0.45 746 247 335 247 2.98 22.39
WBC 45-0.50 0.50 719 247 359 247 2.88 21.58
BBC 52.5-0.40 0.40 674 299 269 331 0.84 -
BBC 52.5-0.45 0.45 652 299 293 331 0.81 -
BBC 52.5-0.50 0.50 632 299 316 331 0.79 -
BBC 50-0.40 0.40 711 284 284 314 0.88 -
Bamboo Particles BBC 50-0.45 0.45 687 284 309 314 0.85 -
BBC 50-0.50 0.50 664 284 332 314 0.83 -
BBC 45-0.40 0.40 775 258 258 285 0.96 -
BBC 45-0.45 0.45 746 258 335 285 0.93 -
BBC 45-0.50 0.50 719 258 359 285 0.89 -
RBC 52.5-0.40 0.40 674 155 269 353 1.35 -
RBC 52.5-0.45 0.45 652 155 293 353 1.31 -
RBC 52.5-0.50 0.50 632 155 316 353 1.26 -
RBC 50-0.40 0.40 711 150 284 342 1.42 -
Rice Husk RBC 50-0.45 0.45 687 150 309 342 1.37 -
RBC 50-0.50 0.50 664 150 332 342 1.33 -
RBC 45-0.40 0.40 775 135 258 307 1.94 -
RBC 45-0.45 0.45 746 135 335 307 1.87 -
RBC 45-0.50 0.50 719 135 359 307 1.80 -

43
Table 4. Experimental results.
Spreading γ28days fc,7days fc,28days E28days
Bio-aggregate type Mixture
(mm) (kg/m3) (MPa) s.d. (MPa) s.d. (GPa) s.d.
WBC 52.5-0.40 248 847 3.19 0.29 4.50 0.41 2.22 0.08
WBC 52.5-0.45 250 836 2.86 0.17 3.92 0.23 2.07 0.03
WBC 52.5-0.50 263 821 2.64 0.24 3.68 0.26 1.86 0.05
WBC 50-0.40 255 905 5.09 0.23 6.07 0.17 2.56 0.04
Wood Shavings WBC 50-0.45 274 872 4.38 0.21 5.45 0.17 2.39 0.06
WBC 50-0.50 275 861 3.80 0.12 4.65 0.10 2.13 0.03
WBC 45-0.40 252 957 6.37 0.35 8.81 0.17 3.24 0.05
WBC 45-0.45 260 945 5.33 0.54 6.35 0.25 2.84 0.04
WBC 45-0.50 275 921 4.94 0.12 5.73 0.36 2.76 0.08
BBC 52.5-0.40 261 652 3.00 0.09 3.39 0.11 1.57 0.09
BBC 52.5-0.45 267 631 2.32 0.16 2.84 0.13 1.50 0.13
BBC 52.5-0.50 272 618 2.26 0.16 2.52 0.07 1.43 0.02
BBC 50-0.40 268 725 2.85 0.06 3.46 0.20 1.92 0.11
Bamboo Particles BBC 50-0.45 270 717 2.45 0.11 3.30 0.13 1.79 0.02
BBC 50-0.50 275 693 2.36 0.07 3.22 0.08 1.68 0.13
BBC 45-0.40 280 795 4.24 0.27 4.57 0.04 2.48 0.20
BBC 45-0.45 286 779 3.88 0.02 4.20 0.18 2.27 0.14
BBC 45-0.50 290 749 2.82 0.17 3.82 0.20 2.21 0.03
RBC 52.5-0.40 245 685 1.58 0.11 1.82 0.09 1.13 0.11
RBC 52.5-0.45 255 659 1.34 0.06 1.68 0.16 1.06 0.05
RBC 52.5-0.50 255 645 1.08 0.11 1.38 0.12 1.03 0.05
RBC 50-0.40 250 722 2.09 0.10 2.28 0.06 1.55 0.09
Rice Husk RBC 50-0.45 265 725 1.75 0.12 1.78 0.13 1.45 0.13
RBC 50-0.50 270 749 1.33 0.05 1.45 0.16 1.58 0.15
RBC 45-0.40 285 902 3.31 0.23 3.51 0.05 1.86 0.20
RBC 45-0.45 290 867 2.76 0.23 2.85 0.17 1.76 0.09
RBC 45-0.50 290 861 2.40 0.24 2.79 0.20 1.88 0.05

44
Table 5. Calibrated values for the mix-design method.
Mixture group k1 k2 k3 k4 k5
WBC 52.5 19.00 425 845
WBC 50 15.00 10.00 7.50 475 905
WBC 45 6.00 560 1000
BBC 52.5 15.00 425 845
BBC 50 10.00 11.00 10.00 475 905
BBC 45 7.00 560 1000
RBC 52.5 19.00 425 845
RBC 50 6.00 12.00 5.00 475 905
RBC 45 5.00 560 1000

45
HIGLIGHTS

- The use of bio-aggregates can improve sustainability of construction sector;

- A fundamental characterization of bio-aggregates is performed;

- A generalized approach for producing workable bio-concretes is presented;

- A novel mix-design method for wood-, bamboo- and rise husk- bio-concrete is proposed;

- The proposed methodology can be extended to other kind of bio-concretes.

Declaration of interests

☒ 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.

☐ The authors declare the following financial interests/personal relationships which may be considered
as potential competing interests: