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Article history: This study reports the use of calcined talc for cementitious products making. The calcination is used to
Received 21 May 2015 enhance the availability of magnesium from talc to react with phosphate for cement phase formation.
Received in revised form 4 July 2015 It is shown that previous calcination of talc leads to products having enhanced mechanical performance
Accepted 13 July 2015
due to the formation of more cement phase than in products based on raw talc. Talc red at 900 C was
Available online 1 August 2015
found to be the one in which magnesium release was maximal. Firing at temperature higher than 900 C
leads to the stabilization of enstatite, which decreased the magnesium availability. The cement phase
Keywords:
is struvite, which was better detected on the X-ray patterns of the products involving red talc. All the
Talc
Calcination
products have very rapid setting time and low shrinkage.
Enstatite 2015 The Ceramic Society of Japan and the Korean Ceramic Society. Production and hosting by
Struvite Elsevier B.V. All rights reserved.
Cement
Compressive strength
http://dx.doi.org/10.1016/j.jascer.2015.07.003
2187-0764 2015 The Ceramic Society of Japan and the Korean Ceramic Society. Production and hosting by Elsevier B.V. All rights reserved.
C.J. Ngally Sabouang et al. / Journal of Asian Ceramic Societies 3 (2015) 360367 361
spectroscopy (SEM/EDS) were used to analyze the products. Setting 30 mA. The diffraction patterns were obtained from 5 to 75 with
time, linear shrinkage, and compressive strength are the mechani- a step of 0.025 .
cal parameters that are evaluated. Infrared spectra were recorded in transmission mode using a
Nicolet Nexus spectrometer. The spectra, recorded from 4000 cm1
to 600 cm1 with a resolution of 1 cm1 , are accumulation of 32
2. Materials and methods
scans.
SEM images are recorded using JEOL JSM-840A and for cou-
A talc from Lamal Pougue in the Boumnybl area at about
pled SEMEDS analysis, an XL 30 microscope by FEI Company is
93 km from Yaound (Center region, Cameroon) was used. The area
used. The samples were carbon-coated prior to analysis for coupled
description is presented in Nkoumbou et al. [16]. The raw material,
SEMEDS.
indexed T0804, was manually ground and sieved at 100 m. The
Setting time was accessed using a Vicat apparatus according to
chemical composition of this talc is given in Table 1. The infrared
the EN 196-3 standard.
and X-ray diffraction characterizations of the raw talc can be found
Measurements of linear shrinkage were done using a Calliper
in Ngally Sabouang et al. [15].
on the hardened mortars aged of 1, 7, 14, or 28 days respectively.
The raw talc is thermally treated using a mufe furnace Car-
Linear shrinkage was calculated using the following equation:
bolite, type CWF 11/5. The temperature rate was set at 5 C/min
and for each ring temperature, the sample is left to soak at the (L0 L) 100
RL =
nal temperature for 2 h. The heating temperature range was from L0
400 C to 1000 C with an increment of 100 C between two con-
secutive heating temperatures. The corresponding red products where L0 is the initial length of specimens at rst days and L is the
are indexed consecutively as T400 up to T1000 prior to infrared length of specimens after a given number of days [15].
spectroscopy and X-ray diffraction analyses. Compressive strength was determined on 28-day cylindrical
Analytical burned magnesia from Rhne-Poulenc, sieved at samples with 60 mm height using an electro-hydraulic press (M&O,
80 m, was used at a dosage of 10% in replacement of part of talc type 11.50, No. 21) with capacity of 60 kN. The samples are submit-
as previously established [15]. As described in Ngally Sabouang ted to a compressive force at average rate of 3 mm/min until the
et al. [15], using X-ray diffraction, the product is mainly made of sample failed according to ASTM C 109 standard test method. The
magnesia with some traces of fortesite and dolomite. compressive strength was calculated using the following equation:
Potassium dihydrogenophosphate was purchased from Alfa
Aesar and used as phosphate ingredient. F
The cement pastes were prepared as follows: = ,
A
In an acidic solution of potassium phosphate, a known amount
of thermally treated talc and, if needed, MgO are added and thor- where F is the failure force and A is the cross-section of the sample.
oughly mixed during 5 min using a M&O mixer. The viscous paste
obtained is used for samples molding and for setting time determi- 3. Results and discussion
nation. The samples were molded using a cylindrical mold having
a diameter of 30 mm and a height of 60 mm. The pastes in the mold 3.1. Characterization of the red talc
are vibrated for 10 min on an electrical vibrating table (M&O, type
202, No. 106) to remove entrapped air bubbles. The samples are The XRPD patterns of the various calcined talc samples are pre-
covered with a polyethylene bag and left for consolidation. The con- sented in Fig. 1. It can be noted that for 400800 C, no signicant
solidated samples are kept at the ambient temperature (2427 C). transformation is observed. At 800 C, a decrease of the d0 0 2 peak
During samples consolidation, linear shrinkage is evaluated every of talc at 9.3 A is observed and was associated with the dehydrox-
7 days up to 28 days. The 28-day samples are used for compressive ylation of the talc in accordance with the work by Villiras [17] in
strength measurement and for SEM/EDX, XRD and FTIR analyses. which dehydroxylation was found to be situated between 800 C
Two series of samples are prepared for each thermally treated and 850 C. At 900 C, the decrease of this d0 0 2 peak is more obvi-
talc sample: a sample without addition of MgO and a sample con- ous, conrming the dehydroxylation of talc. At this temperature,
taining 10% MgO. For each formulation, the ratio water/dry matter the appearance of peaks at 2.85 A, 3.11 A,
and 2.48 A associated to
is 0.2 (in absence of MgO) and 0.4 (in presence of MgO) and the enstatite formation is observed. At 1000 C, the enstatite peaks are
ratio phosphate/talc (or phosphate/talc + MgO) is 0.4. The products better dened. As also reported by Villiras [17], it is observed that
indexations are given in Table 2. during talc ring between 900 C and 1000 C, talc is converted to
Powder X-ray diffraction patterns were recorded using a Philip enstatite. Silica, as a product of dehydroxylation, is not detected
Panalytical PW3710 diffractometer equipped with an iron anticath- given that silica is in amorphous form and will crystallize into
ode operating with a Fe K radiation ( = 1.9373 A) at 40 kV and cristobalite after 1200 C.
Table 1
Chemical analysis of major oxide in the used talc.
SiO2 Al2 O3 Fe2 O3 MnO MgO CaO Na2 O K2 O TiO2 P2 O5 LOIa Total
T0804 51.71 0.61 6.30 0.09 32.08 0.18 <L.D. <L.D.b 0.01 <L.D. 8.01 98.99
a
Loss on ignition.
b
Detection limit.
Table 2
Designation of the various formulations with raw or red talc.
9.3 T
T400 T500 T600 T700
T800 T900 T1000
T700
T600
T500
3.11 T
T400
TB
Transmittance
Intensity (arbitraiy unit)
3235
4.67 T
14.21 C
1.87 T
1638
3553
1618
3.55 C
3478
3414
3678
7.09 C
3660
669
852
938
1016
1051
3600 3100 2600 2100 1600 1100 600
Wavenumber (cm-1)
5 15 25 35 45 55 65 75
2 theta Fig. 2. IR spectra of red talc at various temperatures. TB: raw talc; Tx: red talc at
x C.
9.3 T
2.48 E
2.25 E
2.17 E
9.26 T
TB1000
TB900
Intensity (arbitrary Unit)
3.11 T + E
TB800
3.70 E + S
5 15 25 35 45 55 65 75
2 theta
2.89 E
4.69 T
Fig. 1. X-ray patterns of red talc at various temperatures. TB: raw talc; Tx: red
talc at x C. T, talc; C, chlorite; E, enstatite.
1.95 E
3.15 E
2.34 E
3 S
Intensity (arbitrary Unit)
TB701 temperature (400700 C), one can note that the struvite forma-
TB601 tion in the products based on red talc is more noticeable than
TB501 in raw talc-based products. This is illustrated in Fig. 4c where the
TB401 comparison between the cementitious product based on raw talc
TB001
and the one based on red talc at 400 C, clearly evidences stru-
2.70 S +E
3.10 T
3.24 E
1.86 E
2.89 S
of hydration water favors the reaction of the added MgO and even
2.75
TB1001 tion of the intensity of these bands indicated that magnesium from
TB901
3.11 T + E
TB801
TB001
Intensity (arbitrary Unit)
3.79 S
2.72 S + E
3.73 E+ S
2.89 2.85 S
4.40 E
4.26 S
2.51 E
Transmittance
3553
3233
3478
3414
3677
1638
1618
TB400
670
TB700
TB600
1017
5 15 25 35 45 55 65 75
(b) 2 theta
3600 3100 2600 2100 1600 1100 600
Wavenumber (cm -1)
Intensity (a.u.)
Transmittance
3678
3235
3553
3478
1638
4.24 S
3414
2.71 S
3.32 S
1618
2.9 S
3.56 S
669
TB800
1034
TB900
1247
TB401
851
938
1078
TB001 TB1000
5 15 25 35 45 55 65 75
(c) 2 theta 3600 3100 2600 2100 1600 1100 600
Wavenumber (cm -1)
Fig. 4. X-ray patterns of cementitious products based on talc (raw and red talc at
various temperatures) and 10% of MgO. TB001: using raw talc; TBx: using red talc Fig. 5. IR spectra of cementitious products based on red talc at various tempera-
at x C. T, talc; S, struvite; E, enstatite. tures. TBx: using red talc at x C.
364 C.J. Ngally Sabouang et al. / Journal of Asian Ceramic Societies 3 (2015) 360367
talc takes part in the reaction. The libration of OH from the talc is 0.6
observed at 669670 cm1 ; the decrease of these bands intensities
is another indication that magnesium from Mg OH reacts with the 0.5
2
Transmittance
TB001 0
Brut 500 800 900 1000
TB701
Firing temperature of talc (C)
3553
3235
1615
1638
TB601
3415
3678
TB501 Fig. 8. Compressive strength of cementitious products based on 10% MgO and red
talc.
TB401
1016
669
20
Setting time (Min)
15
Transmittance
10
3678
3235
3553
TB001
3423
669
1618
TB801
851
1017
TB901 5
939
1100
TB1001
Fig. 10. SEM micrographs of cementitious products based on 10% MgO and red talc at 1000 C.
Fig. 11. Coupled SEMEDS analysis of cementitious products based on 10% MgO and red talc at 1000 C.
366 C.J. Ngally Sabouang et al. / Journal of Asian Ceramic Societies 3 (2015) 360367
of the enstatite formed during talc ring. From this conclusion, it increase in cement phase formation, that holds together the par-
was proposed that for the red talc at 800 C, the resulting product ticles, accounts for the increase of the mechanical response. Given
is composed of a cement phase in which the structure is favorable to that the MgO dosage is constant, the differences in the compressive
shrinkage. A formation of an amorphous cement phase is probably strength are assigned to the availability of the Mg from the red
the cause of the observed relatively high shrinkage. talc. It is concluded that as the talc ring temperature increases,
the availability of reacting Mg for the formation of struvite also
3.4. Compressive strength increases. At 1000 C the decrease in compressive strength is asso-
ciated with an increase of enstatite stability that reduced the Mg
The measurements are done on the products with 10% MgO availability. For the red product at 800 C and 900 C, the Mg of
and the results are plotted in Fig. 8. Although the values are low, the enstatite formed is more reactive. As shown by Villiras [17],
an increase from 3.66 MPa to 4.88 MPa is observed with increas- the dissolution experiment of enstatite leads to a maximum Mg2+
ing ring temperature for talc. At 1000 C, a decrease is observed concentration for talc red at 900 C. This is in accordance with
in comparison to the product with the talc red at 900 C. An a maximum availability of Mg from red talc at 900 C that leads
Fig. 12. Elemental map-making on TB1001: (a) for each considered element and (b) reconstitution of the distribution of the various elements analyzed.
C.J. Ngally Sabouang et al. / Journal of Asian Ceramic Societies 3 (2015) 360367 367