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1, January, 921
Mid-infrared (IR) spectra of a series of calcium silicate hydrates (C-S-H) gels synthesised from C3 S in the
presence of magnesium oxide show many similarities with the mid-IR spectra of pure C-S-H gels. However, the
presence of the vibration bands attributed to brucite is observed in all spectra of C-S-H synthesised with MgO,
although only the sample with the highest CaO/SiO2 ratio (1.8) reveals a large shoulder centred at 530 cm1 ,
which has been assigned to the presence of magnesium with a four-fold coordination inserted in the silica chains
of the C-S-H gel. The postulated formation of magnesium silicate hydrates (M-S-H) gel was detected by scanning
electron microscope and energy dispersive analysis of X-rays in some areas of the C-S-H gel with the lowest
CaO/SiO2 ratio (0.66).
25,28
Bonen, simultaneously with the formation of crys-
Introduction
talline brucite and he has also considered the possibility
28
In recent times the incorporation of elements such as of an amorphous brucite formation.
Mg, Na, Cs, K, Sr or even heavy metals during The C-S-H of the cement paste is characterised by a
formation of calcium silicate hydrates (C-S-H) gel has poorly ordered structure with a variable
114 29,30
been the subject of many studies. Some of these composition, CaO/SiO2 (Ca/Si) ratio and [Ca] con-
31
have investigated the incorporation of environmentally trol of the C-S-H gel structure. The stoichiometry of
unfriendly heavy metals into the cement matrix or the most C-S-H gels has been found to be in the range of
3,4,1524 3137
stabilisation of radioactive waste. For this rea- 0.66 , Ca/Si , 2.
son, the study of the mechanisms of interaction be- For a Ca/Si ratio of approximately 0.66, the structure
tween the C-S-H and those elements is of particular of the C-S-H gel presents some analogy with tobermor-
interest. ite, having silicate tetrahedral sheets of SiO2 linear
38,39
There are several reports that deal with the incor- chains associated with an octahedral sheet of CaO.
poration of magnesium into the C-S-H The chain length is assumed infinite. When the Ca/Si
911,2528 11
structure. The relevant study of Pytel con- ratio is increased from 0.66 to 1, calcium appears in
2
siders the incorporation of limited amounts of Mg the interlayer space and the chain length is shortened.
ions into tobermorite, xonotlite and C-S-H. Using Figure 1 shows a typical structure of tetrahedral silicate
40,41
scanning electron microscopy (SEM), Pytel concluded proposed by Klur et al. With a Ca/Si ratio of
that the excess of MgO is hydrated to form Mg(OH)2 , approximately 1.5 and [Ca2 ] 22 mmol/l, Ca(OH)2
and forms magnesium silicate hydrate (M-S-H) of (portlandite) precipitates in equilibrium with the C-S-H
poorly developed structure (MgO/SiO2 1.5) after gel. For this Ca/Si ratio, the structure of the C-S-H is
42
longer periods of hydration. depicted only by silicate dimmers.
The appearance of M-S-H was also postulated by This paper presents the results of a study to investi-
gate the incorporation of magnesium into the C-S-H
gel as a function of the CaO/SiO2 ratio. The C-S-H gel
was synthesised from tricalcium silicate (C3 S) in the
*Institute of Construction Science Eduardo Torroja (C.S.I.C.),
Serrano Galvache 4, 28033, Madrid, Spain.
presence of MgO. Infrared spectroscopy and electronic
(ACR 3430) Paper received 21 January 2003; last revised 12 microscopy techniques were used to follow the Mg
November 2003; accepted 20 July 2004 interaction with C-S-H.
9
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Fernandez et al.
Q2
Ca2octa.non labil
Interlayer space
Q1
Q2p
Fig. 1. Structure of a C-S-H gel for CaO/SiO2 ratios < 1 according to Klur 40
Experimental section CaO 0.5 (Table 1). The C3 S and MgO proportions
were maintained constant but the silica gel content was
Preparation of samples varied.
C-S-H gels with different CaO/SiO2 ratios were The silica gel employed had 99.5% purity, and was
synthesised in the presence of magnesium oxide. The previously dehydrated at 100 8C for 8 h. Magnesium
synthesis was performed using mixes of magnesium oxide was obtained from magnesium hydroxycarbonate
oxide, C3 S and silica gel. CaO/SiO2 ratios ranged from (99.5% purity) previously decarbonated and dehydroxy-
approximately 0.6 to approximately 1.6 and MgO/ lated at 1000 8C for 14 h. The chemical analysis of C3 S
Table 1. Mass of each chemical component mixed for the synthesis of the samples
C3 S: g
MgO: g CaO/SiO2 MgO/CaO
Samples CaO (62.49%) SiO2 (24.92%)
S1 1.5 1.5750 0.3320 0.53 0.49
S2 1.5 1.0419 0.3320 0.72 0.49
S3 1.5 0.6040 0.3320 1.04 0.49
S4 1.5 0.3020 0.3320 1.52 0.49
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Role of magnesium during hydration of C3 S and C-S-H formation
is given in Table 1. The mean diameter of the grains of hydration was performed for 23 days in hydrothermal
C3 S was 15.3 m. conditions at 100 8C inside an autoclave.
Before hydration, and to ensure the homogeneity of
the mixes, the reactants C3 S, silica gel and MgO were Chemical analysis
blended into an agate mortar in the presence of acetone After hydration, the solids and liquids were separated
and stirred for 10 min to facilitate particle dispersion. by filtration. The moist solid samples were dried with
Afterwards the mixes were dried with a heater. acetone to stop further hydration. Chemical analyses of
The homogenised reactants were mixed with distilled Mg, Si and Ca were performed on the liquids and
and decarbonated water at a water/solid ratio of 5. The solids; the results are given in Table 2.
CaCO3
(1490 and 870)
SiOSi bending
(680 and 600)
60
HOH bending
(1650)
40
Silica gel (1100)
OH
(3720)
H 2O
(3460)
20
Internal deformation
C-S-H of TO4 tetrahedra
(970)
(460)
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Fernandez et al.
Mid-IR results
Results
The mid-IR spectra of the four samples are presented
Chemical composition of the solids and the liquids in Figs 2 to 5. In all samples, groups of bands in the
The composition of both the liquid phases obtained range of 8001200 cm1 can be seen, corresponding to
HOH bending
(1650)
60
OH
(3720)
40
H 2O Silica gel (1100)
(3460)
20 C-S-H
(970) Internal deformation
of TO4 Tetrahedra
(460)
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Role of magnesium during hydration of C3 S and C-S-H formation
CaCO3
(1460 and 880)
SiOSi bending of
C-S-H
60
HOH bending
(1650)
OH
(3720)
40
H 2O
the asymmetric and symmetric stretching vibrations of The shoulder centred at 1100 cm1 can be attributed
43
Si-O bonds. One band at about 650 cm1 is attributed to the Si-O stretching vibrations in silica gel.
the Si-O-Si bending vibrations, and the group of bands The characteristic band centred at approximately
at approximately 400500 cm1 correspond to the 970 cm1 (Figs 25) is assigned to the Si-O
43
deformation of the TO4 tetrahedra form (T Si, Al, stretching vibrations of the Si(Q2 ) tetrahedral.
Mg. . .).
Vibration bands are also present at approximately
970 and 1650 cm1 in all samples. A shoulder can be At approximately 3000 to 3800 cm1 , all samples
identified at 1100 cm1 , and it increases in parallel show the stretching vibration of O-H groups in H2 O or
43
with the CaO/SiO2 ratio from S1 to S4. hydroxyl.
The asymmetric stretching of CO3 2 from carbonates An increasing symmetric O-H vibration about
can be observed in the range of 14001600 cm1 . A 3720 cm1 , that increases as the CaO/SiO2 ratio in-
weak shoulder, which corresponds to the out-of-plane creases from S1 to S4, is attributed to brucite (3700
43 4446
bending of appears at approximately 875 cm1 . These cm1 ).
bands are due to a slight carbonation of the samples by Only sample S4 (Fig. 5) displays a Si-O stretching at
the autoclave atmosphere or during the sample prepara- 815 cm1 . Moreover, in the range of deformation of
tion for the characterisation tests. SiO4 tetrahedra (400500 cm1 ), a large shoulder is
The attributions of the vibrations are given in the observed at about 530 cm1 , in detail in Fig. 6. This
following list. shoulder appears clearly for sample S4 and has not
been previously described in mid-IR absorption spectra
The band at 1650 cm1 corresponds to the H-O-H of pure C-S-H gel having a similar CaO/SiO2 molar
43
bending vibration of the molecular H2 O. ratio.
Advances in Cement Research, 2005, 17, No. 1 13
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Fernandez et al.
80
CaCO3
(1460 and
860)
Q1
(815)
SiOSi bending
60
of C-S-H
HOH bending
(1650)
OH
(3720) C-S-H
(970)
20
Internal deformation of
SiO4 tetrahedra
(460)
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Role of magnesium during hydration of C3 S and C-S-H formation
Internal deformation of
MgO4 tetrahedra
(530 cm21)
40
20
S1
S4
Internal deformation of
SiO4 tetrahedra Internal deformation of
(460 cm21) 60 SiO4 tetrahedra
(460 cm21)
40
20
S3
S2
Fig. 6. Mid-IR absorption spectra for the samples S1S4 from 200 to 1000 cm1
protect each C3 S grain by slowing down the progres- samples, some known minerals containing magnesium
sion of the H2 O molecules to the core of C3 S grains. If are also plotted, such as akermanite (Ca2 MgSi2 O7 ),
50
hydrothermal hydration at 100 8C is employed, Masse tremolite (Ca2 Mg5 Si8 O22 (OH)2 ), monticellite
showed that after 14 days, C3 S is almost completely (CaMgSiO4 ), diopside (CaMgSi2 O6 ), merwinite
transformed into C-S-H gel and at 120 8C, the Q0 (Ca3 Mg(SiO4 )2 ), bredigite (Ca7 Mg(SiO4 )4 ). The M-S-
anhydrous (C3 S) disappeared. In the present study, H (MgOSiO2 binary system) and C-S-H are also
hydrothermal conditions at 120 8C were discarded included in order to localise the composition of the
because this temperature allows additional crystallo- samples used in the present study.
50
graphic phases to be formed in presence of MgO as The samples are nearer to the chemical composition
crystalline Mg silicate phases, which would make of C-S-H than M-S-H and this can be deduced from
interpretation of the results difficult. For this reason a Fig. 9. Furthermore, the chemical composition of the
temperature of 100 8C for the hydrothermal hydration S3 and S4 samples are in the area of monticellite,
of C3 S in presence of MgO was considered in present bredigite, merwinite and akermanite.
work.
The Si-O stretching vibrations of C3 S and C2 S do C-S-H gels synthesised in the presence of MgO for
45
not appear in the spectra of hydrated samples, so the CaO/SiO2 ratios , 1.1
anhydrous residue must be very low. The infrared spectra of samples S1 and S2 are rather
A schematic representation of the phase relations in similar to those of the various pure C-S-H gels
43
the system of MgOSiO2 CaOH2 O, including sam- published by Yu et al. and have similar CaO/SiO2
ples S1 to S4, is given in the ternary diagram of Fig. 9. ratios. However, a new band appears in the presence of
In this, the compositions of the hydrated phases have MgO (3720 cm1 ), and this was assigned to
4446
been projected on to the anhydrous base of the system. brucite. The intensity of the sharp symmetric band
Each point has been plotted from the chemical analyses increases as the CaO/SiO2 ratio grows and this suggests
of Table 2. In order to approach the mineralogy of the an increase in brucite content.
Advances in Cement Research, 2005, 17, No. 1 15
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Fernandez et al.
Fig. 7. SEM micrograph in the back-scattered electron mode and EDAX analysis of sample S1
In the presence of MgO, the C-S-H gels formed with C-S-H gels synthesised in the presence of MgO for
a low CaO/SiO2 ratio (, 1) and the replacement of one CaO/SiO2 ratios . 1.1
labile calcium from the interlayer space (Fig. 1) by one The infrared spectra of samples S3 and S4 are
43
magnesium may be possible. The magnesium in the similar to that Yu et al. and again brucite was
interlayer space would have an octahedral coordination. detected (3720 cm1 ). The presence of portlandite was
51 52 53
For instance Tarte, Farmer and Lazarev described not revealed even though the CaO/SiO2 ratio was
in minerals the magnesiumoxygen stretching for octa- higher than 1.5 (S4). The portlandite should be present,
hedral coordination in the range around 300480 cm1 but the expected band was not observed, and conse-
(far-infrared region). No remarkable vibrations of the quently the hydration of C3 S in presence of magnesium
MgO stretching from octahedral co-ordination (300 oxide hinders the precipitation of portlandite.
480 cm1 ) were observed, in the present work. The lack As noted in the results, a large shoulder was ob-
of any observation of a magnesiumoxygen stretching served in sample S3 at 530 cm1 . This vibration is
for octahedral co-ordination does not necessarily imply typical of the range of the TO4 tetrahedra deformation
that the vibration is not present, but might due to poor (T Si, Al, Mg. . .) from 400 to 600 cm1 (Fig. 6).
resolution of the spectrometer in the far-infrared region. The new vibration of S4 is largely shifted from the
However, EDAX results, on sample S1 (CaO/ MgO frequencies for magnesium in octahedral coordi-
5153
SiO2 0.66), suggest that the C-S-H coexists with nation (300480 cm1 ). The appearance of this
brucite (Fig. 7). Some areas that have a high content of shoulder suggests other possibilities.
magnesium and silicon, but low calcium, may be
attributed to M-S-H with a MgO/SiO2 ratio 2.21, (a) The insertion of magnesium in the gap of the Q2p
although with a different stoichiometry to that given by tetrahedron; this possibility should modify the TO4
11
Pytel (1.5). deformation vibration of the Si(Q2 ) tetrahedron, and
16 Advances in Cement Research, 2005, 17, No. 1
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Role of magnesium during hydration of C3 S and C-S-H formation
Fig. 8. SEM micrograph and EDAX analysis of sample S4 for various areas
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Fernandez et al.
Table 3. Analysis by scanning electron microscopy and energy dispersive analysis of X-rays of the different areas of samples
S1 and S4
Sample S1 Sample S4
Molar ratio Grey area Whiteness area Area 1 Area 2 Area 3 Area 4 Global area
CaO/SiO2 0.49 0.08 0.86 1.75 0.80 1.02 1.35
MgO/CaO 0.37 28.60 1.02 0.15 1.75 0.48 0.71
MgO/SiO2 0.18 2.21 0.82 0.26 1.40 0.49
H2O
00 10
Talc, enstatite,
antigorite, forsterite
01 09 and M-S-H
Range of C-S-H gel,
CaO/SiO2 ratio 02 08
between 05 and 18
03 07
Tr
04
em
06
ol
ite
S1
SiO
05
2
05
O
Diopside
Ca
S2
06 04
S3 Akermanite
Monticellite
07 03
ite
ite
S4
in
ig
w
ed
er
Br
08 02
09 01
10 00
00 01 02 03 04 05 06 07 08 09 10
MgO
Fig. 9. Ternary diagram for the MgOSiO2 CaOH2 O system showing the S1S4 samples in the presence of silicates
containing magnesium and/or calcium
induce a shift of the SiO vibration of the Q2 oxygen stretching described in akermanite
53
tetrahedron (Fig. 10(a)). However, this possibility (Ca2 MgSi2 O7 ). The crystallographic structure of
would lead to a vibration largely shifted by about akermanite is constituted by calcium octahedra,
70 cm1 . magnesium and silicon tetrahedra sites (Fig. 10(b)). In
(b) If the vibration is attributed to a deformation of akermanite, the absorption between 600 and 500 cm1
MgO4 tetrahedra (Fig. 10(a)) the incorporation of has been ascribed to the MgO vibrations of the MgO4
53
tetrahedral magnesium in the gap of the Q2p silicon tetrahedron. In fact, the second sphere of co-ordina-
tetrahedra would be equilibrated by calcium, because tion of magnesium tetrahedra coordinated in
54
the Loweinsteins rules exclude the balance by akermanite (Fig. 10(b)) is close to the structure drawn
magnesium (MgOMg). This option is more likely. in Fig. 10(a).
51 52 53
In fact Tarte, Farmer and Lazarev also reported The appearance of a signal at approximately
the vibration of the MgO4 deformation centred at 530 cm1 attributed to tetrahedral coordination of mag-
500550 cm1 , the same range that is found in the nesium does not imply that all of the MgO4 is intro-
present work. duced in the gap of the silica chain, as others sites exist
in C-S-H that could be occupied by magnesium. In a
The actual vibration is also close to the magnesium gel, numerous empty sites exist, but there are few
18 Advances in Cement Research, 2005, 17, No. 1
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Role of magnesium during hydration of C3 S and C-S-H formation
Q2p(Si) H Q0p(Mg)
Ca2 1 Ca2
Ca 2
octa.non labil Q
Gap of Q2p(Si)
H H
Q1
Q2(Si) Ca2 octa. labil
(a)
Q1(SiOSi, 2SiOCa, SiOMg
1
AKERMANITE b
c a
(b)
Fig. 10. (a) Localisation of the magnesium ions into the dreierketten pattern of the C-S-H gel for sample S4. (b) Structure of
akermanite. Spatial group: P421m. Lattice parameters: a 7.8338 A, b 5.0082 A, alpha 90.008, beta 90.008,
gamma 90.008
materials, due their peculiar chemical surrounding, that from EDAX, as high contents of Ca/Si are always
hold tetrahedral magnesium; these materials are detected together with some Mg. In addition, some
55 56 56 57
MgAl2 O4, MgSiN2 , MgAlSiN3, and akermanite. areas in S4 contained high amounts of magnesium.
There is no evidence of the M-S-H formation for However, the EDAX spectrum, which would be repre-
11
high CaO/SiO2 ratio of C-S-H gels, either from IR, or sentative of a M-S-H is not observed.
Advances in Cement Research, 2005, 17, No. 1 19
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Fernandez et al.
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Role of magnesium during hydration of C3 S and C-S-H formation
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