IJE TRANSACTIONS B: Applications Vol. 32, No.

5, (May 2019) 679-684

International Journal of Engineering TECHNICAL

NOTE
Journal Homepage: www.ije.ir

Experimental Study on TGA, XRD and SEM Analysis of Concrete with Ultra-fine
Slag
P. Narasimha Reddy*, J. Ahmed Naqash
National institute of Technology, Srinagar, Jammu & Kashmir, India

PAPER INFO A B S T R A C T

Paper history: The performances of cementitious materials as well as the efficiency of construction are adversely
Received 23 February 2019 affected at high temperatures. Previous studies have already demonstrated that ultra-fine (alccofine)
Received in revised form 25 April 2019 material accelerates the hydration of cement particles and subsequently improves the mechanical and
Accepted 02 May 2019 durability properties of the concrete at normal temperature. Moreover, at higher temperatures the
performance of the concrete with the addition of alccofine is still unknown. This paper presents the
Keywords: effect of analytical properties of concrete with alccofine (25%) as a replacement of cement for various
Alccofine W/B ratios (i.e. 0.38, 0.4 and 0.45). The effect of addition of alccofine dosage on the
Thermogravimetric Analysis thermogravimetric analysis was carried out in which not only mass loss and decomposition of
X-ray diffraction hydration products from concrete with respect to temperature was found but also bound water (%) and
Scanning Electron Microscope calcium hydroxide (%) present in the concrete were determined. From X-ray diffraction it was
observed that alccofine improved the formation of calcium silicate hydrate and calcium silicate
aluminum hydrate in concrete and scanning electron microscope (SEM) analysis showed the formation
of ettringite needles and calcium silicate hydrate in voids which made concrete denser. Therefore, it
was concluded from this study that alccofine can be used as a viable substitute to cement in normal
concrete considering its positive effects on property enhancement and an eco-friendly product.
doi: 10.5829/ije.2019.32.05b.09

1. INTRODUCTION1 replacement of cement or aggregate depending on their

physical and chemical properties [6].
The most regularly utilized building material is According to available literatures, the replacement
concrete, generally made from Portland cement [1]. of cement by industrial by-products which possess
Every material utilized for making concrete affects the pozzolanic nature such as red mud, fly ash [7,8],
environment and gives rise to sustainability issues [2]. metakaolin, silica-fume [9], rice-husk ash [10], mine
However, the manufacture of Portland cement creates a waste , granulated blast furnace slag, etc., have shown
problem such as emission of CO2 (approximately 7 to improved results than the conventional concrete in
8% of total man-made) to the atmosphere and global terms of fresh, mechanical properties and durability
warming [3]. By the addition of a few alternative [11]. Recently, some of the researchers have reported
(pozzolanic) materials, the diverse properties of that the ultra-fine material namely alccofine (ALC) [12-
concrete i.e. strength, workability, durability, and 14], obtained as a by-product from iron ore industry in
permeability may be improved [4]. Researchers have India also possess pozzolanic nature and can be used as
developed different cementing material which can be a fully or partial replacement by weight of cement in
used fully or partially to replace cement which will concrete.
decrease the emission of greenhouse gases [5]. These Chopra and Siddique [15] have studied the effect of
alternative materials can be added to concrete mixes as rush husk ash (RHA) on strength, durable and
microstructural properties were studied. At 15% RHA
*Corresponding Author's Email: narasimha_07phd16@nitsri.ac.in (P.
replacement showed huge formation of calcium silicate
Narasimha Reddy) hydrate and steady state hydration were obtained. Other
investigators have studied the microstructural,

Please cite this article as: P. Narasimha reddy, J. Ahmed Naqash, Experimental study on TGA, XRD and SEM Analysis of Concrete with Ultra-
fine Slag, International Journal of Engineering (IJE), IJE TRANSACTIONS B: Applications Vol. 32, No. 5, (May 2019) 679-684
680 P. Narasimha reddy and J. Ahmed Naqash / IJE TRANSACTIONS B: Applications Vol. 32, No. 5, (May 2019) 679-684

hydration, mechanical properties with metakaolin. The

portlandite changes into calcium silicate hydrate showed
better formation by XRD analysis at 15% of metakaolin
in the concrete. Rathore and Chawda [16] have done an
experimental investigation on high-performance
concrete with the replacement of sand by M-sand and
partial replacement of cement by alccofine and fly ash
for M60 grade of concrete. From the study, they Figure 1. SEM image of cement
conformed that the strength improvement in concrete
with alccofine is higher than that of fly ash. Gayathri et investigation. The physical and chemical properties of
al. [17] conducted research on the performance of AL are given in Tables 1 and 2. Figures 2 and 3 are
concrete with partial replacement with alccofine by shown SEM and EDX images of alccofine.
weight of cement for M30 grade of concrete and she
TABLE 1. Physical properties of Alccofine
observed improvement in the strength of concrete at
15% replacement. Characteristics Test Results
The effect of alccofine on the durability and strength Specific gravity 2.9
properties of the conventional concrete has been 2
Specific surface area [m /kg] 1200
investigated [13] but its effects on the
3
thermogravimetric analysis, X-ray diffraction analysis Bulk density [kg/m ] 680
and scanning electronic microscopy analysis of the Particle Size in Micron
concrete with alccofine have not been well investigated.
D10 1.5
Therefore, this study was designed to assess the
effectiveness of alccofine as constant replacement to the D50 5
cement on the aforementioned properties of mass D90 9
concrete.
TABLE 2. Chemical Properties of AL form EDAX
Results for EDAX
2. RESEARCH SIGNIFICANCE Characteristics of Element
Weight % Atomic %
The Ordinary Portland Cement, which is a major CK 45.69 57.64
constituent of conventional concrete, plays a
significantly important role in attaining the strength OK 35.26 33.39
properties. However, now-a-days manufacturing of Al K 4.01 2.25
cement had become a major source for pollution, which Si K 6.38 3.44
propels the researchers to replace cement by some
Ca K 8.66 3.27
alternative pozzolanic materials that can provide the
desirable mechanical and durability properties to
concrete as well as address the pollution menance.
Previous researchers focused on the use of alccofine in
concrete mix to improve the mechanical and durability
properties of concrete. In the present study, an attempt
has been made to study the effect of alccofine as partial
replacement of cement on analytic properties of
concrete so that their scope to address on thermal and
microstructural properties can be explored.
Figure 2. SEM image of Alccofine
3. MATERIALS

3. 1. Cement In this investigation, OPC 43 grade

was used and it was tested as per Indian standard
specifications [12]. Figure 1 shows the SEM image of
cement.

3. 2. Alccofine AL-1203 was obtained from

Ambuja Cement Ltd, Goa having the specific gravity of
2.9 confirming to ASTM C989-1999 was used in entire Figure 3. EDX image of alccofine
 P. Narasimha reddy and J. Ahmed Naqash / IJE TRANSACTIONS B: Applications Vol. 32, No. 5, (May 2019) 679-684 681

3. 3. Aggregates Natural river sand with specific 4. 3. 2. X-Ray Diffraction Analysis (XRD) XRD
gravity 2.68 was used conforming to zone II as per is an important method used for the quantitative and
Indian standard specification. The crushed stone angular qualitative analysis of hydrated cement concrete
aggregate was used as coarse aggregate with the specific samples. The X-Ray diffraction is based on Bragg’s
gravity of 2.79. The maximum size of the aggregate was law. By using X-Ray diffraction test results, a graph
limited to 20 mm. between the angle at which the wave was diffracted and
intensity of X-ray was determined. The XRD test was
3. 4. Water In this investigation, ordinary tap water conducted on samples on the 28th day. The
available in campus was used for all concrete mixes. diffractometer with CuKu source having a wavelength
of χ = 1.54À at the scanning speed of 2s/ step and the
diffraction angle between 7° and 60° was employed for
4. DATA, AND EXPERIMENTAL INVESTIGATION test conduction.

4. 1. Mix Proportion The ingredients of concrete 4. 3. 3. Scanning Electronic Microscope Analysis

i.e. Cement, coarse aggregate, and fine aggregate were (SEM analysis) SEM analysis was used to
mixed in the proper proportion by addition of water as determine the microstructure of the hardened concrete
shown in Table 3. Alccofine was added to the mixes as with and without alccofine. The concrete samples were
a replacement of cement by 25% mass. taken in a small size of 5 mm, which consist of fine
aggregate and mortar.
4. 2. Preparation of Sample Mixing procedure and
curing method was kept the same for TGA, XRD and
SEM samples. For TGA and XRD, the samples were 5. RESULTS AND DISCUSSION
ground and sieved through 63 lm sieve. To stop
hydration and to remove physically bound water the 5. 1. Thermogravimetric Analysis From
solvent exchange method was adopted using acetone. A thermogravimetric analysis results, the mass loss along
100 mL of acetone was added to 30 g of the sieved with the decomposition of all components with
sample in a plastic bottle and mixed vigorously by hand temperature was found. The thermogravimetric analysis
for about 3 min. Excess acetone was drained out and the showed that significant weight loss can occur in many
process was repeated. The samples were then dried ways. The primary effect from 25ºC to 100ºC had to do
overnight in an oven at 40⁰C temperature. The dried with the residual pore water which evaporated from
samples were collected and stored in a sealed plastic capillary pores [13]. In this stage, the weight loss
container till the time of testing. depended upon the adsorbed water, interlayer water and
capillary pores. The second effect from 100 to 450ºC
4. 3. Methods had to do with dehydration of calcium silicate hydrates,
4. 3. 1. Thermogravimetric analysis Total of ettringite and C-A-H. The third at about 475-750ºC is
twelve samples (with and without alccofine) were due to the decomposition of calcium hydroxide formed
studied by Thermogravimetric analysis. Small samples during hydration as shown in Equation 1 [18].
were taken from the concrete cube and heat was applied
from 25ºC to 1000ºC in a thermal analyzer with a rate Ca(OH)2 → CaO + H2O (1)
of heating 10ºC/min. From TGA experiment, weight The last weight loss effect around 800ºC can be
losses with respect to increasing temperature and peak attributed to decarbonization of CaCO3 as shown in
temperature for the decomposition of hydrates like Ca Equations (2) and (3).
(OH)2, calcite, calcium silicate hydrate and C-A-S-H.
Ca(OH)2+CO2 → CaCO3 + H2O (Carbonation) (2)
TABLE 3. Mix proportions for trail mixes
S.No M C AL FA CA W/B CaCO3 → CaO + CO2 (Decarbonation) (3)
1 NM1 438.13 0 644.59 1118.42 0.45 Figure 4 shows the decomposition of all hydration
2 AF1 328.59 109.53 644.59 1118.42 0.45 compounds in the temperature range of 23-800°C and
Figure 5 shows the weight loss of normal and high
3 NM2 492.90 0 610.55 1106.06 0.40 dosage alccofine concrete at different water to binder
4 AF2 369.67 123.22 610.55 1106.06 0.40 ratios with respect to temperature [14]. It can be clearly
seen from Figure 5 that the percentage of weight loss in
5 NM3 518.84 0 595.98 1098.62 0.38 alccofine concrete is less than that of the normal
6 AF3 388.18 155.65 595.98 1098.62 0.38 concrete. From Equations 4 and 5, the content of
Units: M-Mix, C-Cement, AL-Alccofine, FA- Sand and CA-Gravel
calcium hydroxide and bound water were calculated as a
W/B-Water to binder ratio in kg/m3 percentage of the weight at 580°C [19] as follows:
682 P. Narasimha reddy and J. Ahmed Naqash / IJE TRANSACTIONS B: Applications Vol. 32, No. 5, (May 2019) 679-684

Calcium hydroxide (%) = x x 100 (4)

The molecular weight of Calcium hydroxide is 74 and

that of water is 18.
Bound water (%) = x 100 (5)

From obtained results percentage of calcium hydroxide

was more in normal concrete but the percentage of
bound water had more values in high dosage alccofine
concrete compared to normal concrete [20] as shown in Figure 7. Bound water (%) of the concrete for various W/B
Figures 6 and 7. The percentage of calcium hydroxide ratio
was less in alccofine concrete because alccofine reacts
with calcium hydroxide to form additional CSH gel
whereas no such entity exists in normal concrete to react 5. 2. X-Ray Diffraction Analysis (XRD) XRD
with the same thereby increasing the percentage of analysis is a one of the method to find mineral
calcium hydroxide in normal concrete [21]. composition like calcium silicate hydrate (C-S-H),
calcium aluminosilicate hydrate (C-A-S-H), portlandite
(Ca(OH)2) and ettringite present in the concrete [22].
Figures 8, 9 and 10 shows the peak intensities for
control and alccofine concrete at different water to
binder ratio (i.e. 0.38, 0.4 and 0.45).
The intensity of calcium hydroxide (Ca(OH)2) in the
presence of alccofine at 2θ= 20.64 has increased
compared to normal concrete for all water to binder
ratios. Formation of Ca(OH)2 is more in normal concrete
compared to alccofine concrete [14]. Further, the
intensity of ettringite in the presence of alccofine at
Figure 4. DSC curves of the concrete for different water to 2θ=22.87 has decreased compared to without alccofine.
binder ratios
The peak intensity of calcium silicate hydrate at
2θ=26.46 has increased more in the presence of
alccofine compared to normal concrete and the intensity
of calcium aluminosilicate hydrate is more in normal
concrete at 2θ=28.29 indicating rapid hydration. The
formation of CSH is more in with high dosage alccofine
concrete due to Ca(OH)2 converted to secondary CSH
and therefore enhancing strength of the concrete[18-24].

Figure 5. Percentage of weight loss curves of the concrete for

different W/B ratio

Figure 8. XRD analysis of the concrete at W/B = 0.45

Figure 6. Calcium hydroxide (%) of the concrete for various

W/B ratio Figure 9. XRD analysis of the concrete at W/B = 0.40
 P. Narasimha reddy and J. Ahmed Naqash / IJE TRANSACTIONS B: Applications Vol. 32, No. 5, (May 2019) 679-684 683

From the thermogravimetric analysis, alccofine concrete

was found to have more bound water and less calcium
hydroxide (due to pozzolanic action) with respect to
normal concrete at different water to binder ratio. It was
also found that alccofine concrete had less weight loss
and decomposition of hydrates compared to normal
concrete thereby making it more stable. From XRD and
SEM analysis, alccofine decreased the porous
Figure 10. XRD analysis of the concrete at W/B = 0.38 microstructure and improved the formation of calcium
silicate hydrate and calcium silicate aluminum hydrate
in the concrete. Hence, from the results obtained in this
5. 3. Scanning Electronic Microscope Analysis
study it can be concluded that substituting the cement in
SEM images give information regarding the
concrete by alccofine is a feasible mean considering
microstructure and surface morphology of calcium
enhanced properties and eco-friendly nature of concrete.
silicate hydrate and ettringite in concrete. It was
observed that alccofine concrete gives less porous
structure due to the formation of needles in voids
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18. BIS. 8112, Indian Standard 43 Grade Ordinary Portland

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Experimental Study on TGA, XRD and SEM Analysis of Concrete with TECHNICAL
NOTE
Ultra-Fine Slag
P. Narasimha Reddy, J. Ahmed Naqash
National institute of Technology, Srinagar, Jammu & Kashmir, India

PAPER INFO

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