Available online at www.sciencedirect.

com

Construction and Building

Construction and Building Materials 22 (2008) 20782086

MATERIALS
www.elsevier.com/locate/conbuildmat

Cement-lateritic gravels mixtures: Microstructure and strength characteristics

Younoussa Millogo a, Mohamed Hajjaji
a b

b,*

, Raguilnaba Ouedraogo a, Moussa Gomina

riaux (LPCTM), UFR/Sciences Exactes et Applique es, Laboratoire de Physico-Chimie et de Technologie des Mate de Ouagadougou, 03 B.P. 7021 Ouagadougou 03, Burkina Faso Universite ` nes dInterfaces, De riaux Naturels et Phe nome partement de Chimie, Faculte de Sciences Semlalia, Equipe de Physico-Chimie de Mate Cadi Ayyad, Boulevard Prince My Abdellah, B.P. 2390, Marrakech, Morocco Universite c chal Juin, 14050 Caen Cedex 4, France Laboratoire CRISMAT UMR 6508 CNRS/ENSICAEN, 6 Bd Mare Received 15 December 2006; received in revised form 11 July 2007; accepted 23 July 2007 Available online 4 September 2007

Abstract Microstructure of cement-lateritic gravels mixes, containing up to 8 wt% cement, was investigated by means of X-ray diraction, infrared spectrometry, dierential thermal analysis, scanning electron microscopy and energy dispersive spectrometry. Also, strength characteristics of the mixtures were measured. The results show that cement admixtures resulted in the formation of 1.4 nm-tobermorite, ettringite, iron oxyhydroxide, portlandite and calcite. The increasing amount of tobermorite, due to the increase of the cement content, was attended with a noticeable reduction of particles segregation. In addition, its marked crystallization, observed for the high curing time (28 days), contributed to the improvement of the mechanical strength. As regards the application aspect, the results show that cement amended lateritic gravels are convenient for base course construction. 2007 Elsevier Ltd. All rights reserved.
Keywords: Lateritic gravels; Cement mixes; Microstructure; Mechanical strength; Base course

1. Introduction Lateritic soils are widespread materials in tropical and subtropical African countries. They are required for road construction. However, the road sections built with raw lateritic soils are the subject of deterioration because of rain erosion and trac intensication [15]. The viability of roads consisting of lateritic soils is proven to be dependent on the chemical and mineralogical compositions as well as the mechanical characteristics of these raw materials [4]. To improve the latter properties, additions of lime, cement, ash y, silica fume and vegetable bres were tested [2,3,510]. If the physical parameters of amended argillaceous lateritic soils from some West African countries have been evaluated, a little attention is paid
*

to the investigation of their microstructure as well as to the study of the lateritic gravels of Burkina Faso, which are lean clay materials [2,3,5,6,911]. This work is devoted to the study of the microstructure and the determination of strength characteristics of cement modied lateritic gravels from Burkina Faso. The potential use of these amended materials for road construction is discussed. 2. Materials and experimental procedures 2.1. Materials The mineralogical and chemical compositions of the concerned lateritic gravels, taken from Sapouy (Burkina Faso), are given in Table 1. The values of some physical properties of these materials are gathered in Table 2. Comments on these characteristics are reported elsewhere [12].

Corresponding author. Tel.: +212 24 43 46 49; fax: +212 24 43 74 08. E-mail address: Hajjaji@ucam.ac.ma (M. Hajjaji).

0950-0618/$ - see front matter 2007 Elsevier Ltd. All rights reserved. doi:10.1016/j.conbuildmat.2007.07.019

Y. Millogo et al. / Construction and Building Materials 22 (2008) 20782086 Table 1 Chemical and mineralogical compositions (in wt%) of the concerned lateritic gravels Chemical composition: SiO2 56.19 Mineralogy:
a

2079

Al2O3 10.10

Fe2O3 16.09 Quartz 42

MgO 0.05

CaO 3.24 Goethite 15

MnO 1.68

Na2O 2.01 Hematite 3

K2O 0.07

TiO2 1.39 Rankinite 6

CuO 0.11

L.O.I. 8.14 Balancea 8

Kaolinite 26

Constituted mainly of illite and organic matters.

Table 2 Geotechnical and mechanical characteristics of the used lateritic gravels Particles size distribution (wt%) < 2 mm (Skeleton) 28
a b c d e f g

Atterberg limits (%) <2 lm (Clays) 5 wLa 22.5 wP 12

b

Blue methylene value MBV (g/100 g) 0.17

d

Modied proctor OMC (%) 6.6

e

California bearing ratio

f

<0.425 mm (Mortar) 18

<80 lm (Fine particles) 10.5

PI

MDD (kN/m3) 21.7

CBRg (%) 43

10.5

Liquid limit. Plasticity limit. Plasticity index. 100 g is the sample weight. Optimum moisture content. Maximum dry density. CBR at 95% of MDD.

The used cement (Portland (CPA 45)) is supplied by Diamond Cement in Burkina Faso. Its mineralogical and chemical compositions and some of its physical characteristics are gathered in Table 3. 2.2. Experimental procedures The studied mixtures consisted of cement (up to 8 wt%) and lateritic gravels. For samples preparation, the above mentioned materials were oven-dried at 105 C for 24 h, manually mixed, for preventing the grain size change, and stored in hermetic plastic bags in order to ovoid moisture contamination. The plasticity index (PI) and the methylene blue value (MBV) of the mixtures were evaluated according to the NF P94-051 [13] and NF EN 933-9 norms [14], respectively. The optimum moisture content (OMC) and the

maximum dry density (MDD), and the California Bearing Ratio (CBR) of mixes were determined in conformity with the NF P94-093 [15] and NF P94-078 [16] standards, respectively. For the CBR measurements, dierently treated samples were punched with a universal press (SEDITECH apparatus). The grain size distribution was realized by dry sieving as well as by sedimentation, according to the NF P18-560 [17] and NF P94-057 [18] standards, respectively. The former method was used for the classication of coarse particles (>80 lm in size), when the second one was applied for tiny grains (<80 lm). The mechanical tests were realized on cylindrical testpieces of mixtures, which were moulded in CBR moulds at the optimum Proctor modied, and kept in room temperature for 7, 14 and 28 days. They were performed with a universal press and carried out according to the NF P18406 [19] norm for the compressive strength and the NF

Table 3 Chemical and mineralogical compositions (in wt%) and some physical properties of the used cement Chemical composition: SiO2 20.12 Al2O3 5.73 Fe2O3 4.06 MgO 1.18 CaO 64.82 P2O5 0.39 SO3 2.68 Na2O 0.08 K2O 0.17 F.La 0.80 I.Rb 0.28 L.O.I. 0.27

Mineralogy:

C3S 55.70

C2S 15.68

C3A 8.31 Apparent density (g/cm3) 1.06

C4AF 12.34 Setting time (h) 3

Physical properties:

Specic gravity (g/cm3) 3.02

Free lime.

2080

Y. Millogo et al. / Construction and Building Materials 22 (2008) 20782086

P18-408 [20] standard for the tensile strength. As concerns the compressive strength determination, the test-piece experienced an increasing load until rupture. Knowing the ultimate load (Fmax, kN) and the average cross-section area of the test piece (S, cm2), the magnitude of the compressive strength (MPa) is determined according to the relation: (10Fmax)/S. For the tensile strength, the loading rate was 0.05 MPa/s and the magnitude, in MPa, was found by the formula: (0.637P)/(d h), where P (106 N) is the applied charge, d (m) and h (m) are the diameter and the height of the cylindrical test-piece. The nature of crystalline phases in the prepared samples was identied by means of a Philips XPert MPD diractometer equipped with a copper Ka radiation (Ka = ). The infrared examinations were done on discs 1.5418 A consisting of 1 mg of cement-lateritic gravels samples, taken from the above-mentioned mixtures, and 150 mg of potassium bromide (KBr). They were performed by means of a Nicolet 510FT-IR spectrometer, operating in the range 4000400 cm1. The thermal changes of the mixes were evidenced by means of a LabsysSetaram apparatus, functioning at a heating rate of 10 C/min and under N2 atmosphere. The microscopic examinations were done on carboncoated pieces taken from the above-mentioned cylindrical samples, using a Jeol JSM 5500 scanning electron microscope, equipped with a Falcon EDAX analyser. The elemental quantitative analyses were performed without standards (ZAF method). The maximum resolution was around 3.5 nm. 3. Results and discussion 3.1. Mineralogical and microstructural characterization As can be derived from the X-ray diractograms of Fig. 1, cement additions gave way to the formation of ettringite, calcite and portlandite (CaO H2O or CH). As compared to CH, the two former compounds occurred in low cement content samples. X-ray reections assignable to 1.4 nm-tobermorite became evident with the increase of the cement amount. To evidence the eventual presence of amorphous compounds, mixes of cement-lateritic gravels were subjected to thermal and IR spectroscopy analyses. As regards the thermal results (Fig. 2), the endothermic eects at around 80, 350, 530 and 567 C are linked to dehydration water, loss of crystallization water of goethite, deshydroxylation of kaolinite and to the transformation of quartz a to b, respectively. The weak thermal eect at 150 C is assignable either to CSH (CaO SiO2 H2O) type tobermorite and ettringite [2124], when the one at 385 C is attributable to the deshydroxylation of portlandite. Concerning the infrared investigations (Fig. 3), the spectra displayed bands relevant to quartz, kaolinite, goethite and hygroscopic water. Bands associated with calcite and carbon dioxide are also present. It is worth noting that the marked intensication of the broad

T Intensity (a.u.)

I K

Q Q E GK Q Q T G H H I K I Q C I T Q E Q Q K K K R K K R Q T I C K G (b)

(a) 10 20 30 40 50 60 70 2

Q I K E G Intensity ( a.u.)

Q Q GH Q C I K T K R CP K P Q K I R I I Q Q QI R R T P Q E Q R R (d) C Q R

(c) 10 20 30 40 50 60 70 2

Fig. 1. X-ray diraction patterns of the lateritic gravels (a) and cement amended samples (b: 2, c: 3 and d: 8 wt% cement). K: kaolinite; I: illite; Q: quartz; G: goethite; H: hematite; T: tobermorite, E: ettringite; P: portlandite; and C: calcite.

Quartz transformation ( to ) Kaolinite dehydroxylation G Dehydration T+E CH

(d)

(c) (b)

Endo

(a)

200

400

600

T(C) 800

Fig. 2. Thermograms of the basic raw material (a) and its cement mixes (b: 2, c: 3 and d: 8 wt% cement). G: goethite; C: calcite; CH: portlandite; E: ettringite; and T: tobermorite.

band at 3400 cm1, which is commonly attributed to hydration water, may be taken as an indication of the presence of CSH (tobermorite), which presence is revealed by the band at 670 cm1 [25,26].

Y. Millogo et al. / Construction and Building Materials 22 (2008) 20782086

2081

Si-O (K) Si-O-Si K Al-Al-OH (K) Si-O(K) Si-O(Q) C T G

(d)

(c)

(b)

(a)
H2 O

1900

1700

1500

1300

1100

900

700

500

300

100

Wavenumber (cm-1)

Al-Al-OH CO2

(d)

H2O+T

(b)

(a)

3800 3600 3400 3200 3000 2800 2600 2400 2200 2000

Wavenumber (cm-1)
Fig. 3. Infrared spectra of the lateritic gravels (a) and mixes containing 2 (b), 3 (c) and 8 wt% cement (d).

It may be noticed that the endothermic eect relevant to the deshydroxylation of kaolinite experienced a slight decrease with cement additions. This is likely linked to the pozzolanic reaction involving clay minerals [10]. Segregated particles of quartz (Fig. 4a; Zones A and B) and kaolinite (Fig. 4b; Zone C) were identied in cementfree samples. However, in lower cement content samples, agglomerated particles developed (Fig. 4c) and an iron oxyhydroxide, looking like FH3 (Fe2O3 3H2O), was discriminated (Fig. 4c; Zone D) [27]. The agglomeration seems to be the consequence of occulation, which resulted of the cation exchange of compensating charges of the basic material and Ca2+ ions, deriving from cement hydration [10]. Small particles, which consisted mainly of calcium and sulphur, were distinguished (Fig. 4d; Zone E). Apparently, these correspond to ettringite (C =S 1:77), which could be developed from the aqueous reaction between gypsum and C3A (3CaO Al2O3). The increase of the

cement content led to the occurrence of sulphurcalciumrich zones constituting of portlandite and/or calcite, ettringite, and tobermorite (Fig. 4d; Zone F) [28,29]. Referring to some authors [26,30,31], the latter CSH could be originated from the hydration of the components of cement (C3S and C2S (2CaO SiO2)), but its partial formation from the pozzolanic reaction involving clay minerals and portlandite is plausible. For higher cement content (e.g., 8 wt% cement) (Fig. 4e and f, Zones G and H), ettringite is rarely encountered. Based on reported results [32], it appears that the reaction between SO2 4 ions, provided by gypsum, and C3A for forming ettringite became less signif icant as compared with the xation of SO2 4 on CSH phase. The sulphate xation should be favoured because of the alkalinity of the medium (pH 11.41). On the other hand, it may be remarked that as a result of higher cement content, precipitates of tobermorite became abundant (Fig. 4f; Zone H).

Absorbance(a.u.)

Absorbance (a.u.)

2082

Y. Millogo et al. / Construction and Building Materials 22 (2008) 20782086

Fig. 4. Typical SEM micrographs and EDS analyses relevant to the concerned samples. (a, b): lateritic gravels; (c) : 2 wt% cement; (d): 3 wt% cement; (e, f): 8 wt% cement.

3.2. Physical characteristics As can be deduced from the grain size distribution curves of Fig. 5, the amounts of skeleton (<2 mm), mortar

(<0.425 mm) and ne particles (802 lm) increased by about 1.7-fold as a result of cement additions. In contrast, the amount of the clay-sized fraction (<2 lm) experienced a slight decrease, likely because of its implication in the

Y. Millogo et al. / Construction and Building Materials 22 (2008) 20782086

2083

Fig. 4 (continued)

above-mentioned processes, namely agglomeration and pozzolanic reaction. As a consequence of the reduction of the clay fraction, the plasticity index and the methylene blue value decreased (Fig. 6).

Cement additions also have an eect on the optimum moisture content and the maximum dry density (Fig. 7). The evolution of the former property is linked to an increasing cement anity for water. In fact, the raising of

2084

Y. Millogo et al. / Construction and Building Materials 22 (2008) 20782086

100

Percentage passing (wt.%)

0; 4;

2; 6;

3; 8 wt.% cement

80 60 40 20 0 10 1 0.1

Particle size (mm)

Fig. 5. Particle size distribution curves relevant to the concerned samples.

of the aggregation phenomenon due to cement additions, the volume of particles increases and consequently MDD decreases. On the other hand, it may be noticed that the obtained values for OMC (7.28.2%) and MDD (2.16 2.1 g/cm3) lay in the required ranges for base course materials [3]. The variation of CBR versus cement content is reported in Fig. 8. The CBR increasing is due to the continuous development of tobermorite, which is known as a cementitious compound. On the other hand, the higher values of CBR, relevant to the water immersed fresh specimens, may be interpreted in terms of an uninterrupted process of cement hydration. Corollary, for water immersed dry samples, such process could not keep on since the required setting time of cement is around 3 h. The observed evolutions of CBR are inconsistent with the results reported in reference [2]. The discrepancy may be linked to the

PI (%)
PI 10.5

MBV(g/100g) MBV
0.16

600

a
450

CBR (%)

10.0

0.12

300

9.5

0.08
150

8
0 2 4 6 8

Cement content (wt.%)

Fig. 6. Variations of the plasticity index (PI) and methylene blue value (MBV) vs. cement content.

Cement content (wt.%)

Fig. 8. Evolution of California Bearing Ratio (CBR) of 4 days water immersed samples (freshly prepared (a) and 3 days dried (b)) as a function of cement content.

8.5

MDD

OMC

2.18 8.0
3 MDD (g/cm )

7.5

Compressive strength (MPa)

2.16

7 days 6

14 days

28 days

OMC (%)

2.14 2.12 2.10 0 2 4 6 8

7.0

6.5

Cement content (wt.%)

Fig. 7. Variations of the optimum moisture content (OMC) and maximum dry density (MDD) against cement additions.

cement content should be accompanied by an increasing water demand for the dissociation of portlandite. As regards the variation of MDD, it is believed that because

Cement content (wt.%)

Fig. 9. Eects of cement additions and curing time on the evolution of the compressive strength of lateritic gravels samples.

Y. Millogo et al. / Construction and Building Materials 22 (2008) 20782086

2085

7 days
0.4

14 days

28 days

Tensile strength (MPa)

0.3

versitaire de la Francophonie (A.U.F.) for their nancial support. The authors are grateful to Profs Thomas Armbr and uster (University of Bern; Switzerland), Karfa Traore Abdelkader Outzourhit as well as to Aziz Khalfaoui, and Rachid El Moutamanni for their helps. References
[1] Gidigasu MD. Lateritic soil engineering. The Netherlands: Elsevier Science Amsterdam; 1976. canique dune couche de base en [2] Messou M. Comportement me ritiques ame liore s au ciment : cas des routes en Co te graveleux late ` se de Doct-Ing en Ge ` l Ecole Nationale des nie Civil a dIvoire. The es, Paris; 1980. Ponts et Chausse ritiques en technique [3] Bagarre E. Utilisation des graveleux late ` re. ISTED 1990. routie ra M, Chiasson PA, Maiga MS. Les graveleux [4] Tockol I, Massie me ritiques dans les pays du sahel: Cas des routes non reve tues. 7e late ` s International de AIGI, Rotterdam, Holland; 1994. Congre [5] Attoh-Okine NO. Lime treatment of laterite soils and gravelsrevisited. Construct Build Mater 1995;9(5):2837. rites et graveleux late ritiques. Laboratoire Central des [6] Autret P. Late es, France; 1983. Ponts et Chausse [7] Akoto BKA. The eect of repeated loading on the ultimate unconned compressive strength of a lime stabilized laterite. Eng Geol 1986;23:12535. [8] Attoh-Okine B. Stabilization eect of locally produced lime on selected lateritic soils. Construct Build Mater 1990;4(2):8691. [9] Osula DOA. Lime modication of problem laterite. Eng Geol 1991;30:14154. [10] Osula DOA. A comparative evaluation of cement and lime modication of laterite. Eng Geol 1996;42:7181. [11] Simon AB, Giesecke J, Bidlo G. Use of lateritic soils for road construction in north Dahomey. Eng Geol 1973;7:197218. K, Ouedraogo R, Kabore K, Blanchart P, [12] Millogo Y, Traore Thomassin JH. Geotechnical, mechanical, chemical and mineralogical characterization of lateritic gravels of Sapouy (Burkina Faso) used in road construction. Construct Build Mater, in press, doi:10.1016/j.conbuildmat.2006.07.014. termination des limites dAtterberg; Mars 1993. [13] NF P94-051, De terminer les caracte ristiques ge ome tr[14] NF EN P933-9, Essais pour de ` ne; Aou thyle iques des granulats. Essai au bleu de me t 1999. termination des re fe rences de compactage dun [15] NF P94-093, De riau; Octobre 1999. mate ` s immersion- Indice CBR imme diat[16] NF P94-078, Indice CBR apre diat; De cembre 1992. Indice Portant Imme trique par tamisage; Octobre [17] NF P18-560, Analyse granulome 1978. trique des sols, Me thode par [18] NF P94-057, Analyse granulome dimentation; Mai 1992. se tons Essai de compression; De cembre1981. [19] NF P18-406, Be tons Essai de fendage; De cembre 1981. [20] NF P18-408, Be [21] Rojas MF, Sanchez de Rojas MI. The eect of high curing temperature on the kinetics in MK/lime and MK-bended cement matrices at 60 C. Cement Concrete Res 2003;33:6439. [22] Assal HH. Inuence of silica fume on the properties of red then water cured lime-rich clay bricks. Silic Ind 2003;68(56):5560. [23] Kolias S, Kasselouri-Rigopoulou V, Karahalios A. Stabilisation of clayey soils with high calcium y as hand cement. Cement Concrete Compos 2005;27:30113. [24] Lanas J, Sirera R, Alvarez JI. Compositional changes in lime-based mortars exposed to dierent environments. Thermochim Acta 2005;429:21926. [25] Dutta DK, Bordoloi D, Prakash C. Hydratation of portland cement clinker in the presence of carbonaceous material. Cement Concrete Res 1995;25:1095102.

0.2

0.1

0.0

Cement content (wt.%)

Fig. 10. Variation of the tensile strength of dierent aged samples against cement admixtures.

dierence in the clay minerals amounts: because of their lower contents, the clay minerals pozzolanic reactions in the concerned lateritic gravels are less quantitative as compared with those happened in clay-rich laterite used by Messou [2]. The variations of the compressive and tensile strengths of dierently cured samples as a function of cement content are shown in Figs. 9 and 10, respectively. The observed increase of both strengths is chiey attributed to the formation of tobermorite, which crystallization is time dependent. Since the compressive strengths are in the range 1.45 3.1 MPa and the CBR values are higher than 160%, the studied cement-lateritic mixtures are suitable for base course construction [3]. 4. Concluding remarks Cement additions to lateritic gravels led to the formation of a homogeneous microstructure and improved the mechanical strength. These positive impacts are mainly related to the development of 1.4 nm-tobermorite, which derived principally from cement hydration. Likely because of their minor amounts, the adverse eect of calcite and portlandite on the mechanical properties was insignicant. On the other hand, basing on the reported data relevant to the use of lateritic gravels in road construction [3], the measured physical magnitudes allow to conclude that the concerned cement amended lateritic gravels are convenient for base course manufacture. For economic considerations, as small a quantity as 2 wt% is sucient for this kind of construction. Acknowledgements timent et des Thanks to the Laboratoire National du Ba Travaux Publics du Burkina Faso and the Agence Uni-

2086

Y. Millogo et al. / Construction and Building Materials 22 (2008) 20782086 [30] Mitchell DRG, Hinczak I, Day RA. Interaction of silica fume with calcium hydroxide solutions and hydrated cement pastes. Cement Concrete Res 1998;28(11):157184. s, [31] Viallis-Terrisse H. Interaction des silicates de calcium hydrate principaux constituants du ciment, avec les chlorures dalcalins. ` se de Doctorat de lUniversite de Analogie avec les argiles. The Bourgogne (France), UF des Sciences et Techniques; 2000. [32] Divet L, Randriambololona R. Delayed ettringite formation: the eect of temperature and basicity on the interaction of sulphate and CSH phase. Cement Concrete Res 1998;28(3):35763.

[26] Yu P, Kirkpatrick RJ, Poe B, McMillan PF, Cong X. Structure of calcium silicate hydrate (CSH): near-, mid-, and far-infrared spectroscopy. J Am Ceram Soc 1999;82(3):7428. es Ouvrages dArt du Re seau des L.P.C., Lyon; 13 Avril 2005. [27] Journe [28] Klimesch DS, Ray A. Hydrogarnet formation during autoclaving at 180 C in unstirred metakaolin-lime-quartz slurries. Cement Concrete Res 1998;28(8):110919. [29] Gleize PJP, Muller A, Roman HR. Microstructural investigation of a silica fume-cement-lime mortar. Cement Concrete Compos 2003;25:1715.