Construction and Building Materials 213 (2019) 209–215

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Construction and Building Materials

journal homepage: www.elsevier.com/locate/conbuildmat

Study on the pozzolanic reaction of clay brick powder in blended cement

pastes
Jiahu Shao a,b, Jianming Gao a,b,⇑, Yasong Zhao a,b, Xuemei Chen a,b
a
Southeast University, School of Materials Science and Engineering, Nanjing 211189, China
b
Jiangsu Key Laboratory of Construction Materials, Nanjing 211189, China

h i g h l i g h t s

 The pozzolanic reaction of CBP contributes to the compressive strength of mortars.

 Hydration products of blended pastes contain CH, C-S-H, C-A-H and C-A-S-H gels.
 The pozzolanic reaction of CBP mainly occurs between 60 days to 90 days.

a r t i c l e i n f o a b s t r a c t

Article history: Recycled clay brick powder (CBP) from waste clay bricks was utilized as a supplementary cementitious
Received 29 August 2018 material to partially replace cement to prepare cement pastes or mortars. The compressive strength,
Received in revised form 24 March 2019 hydration products and microstructure of these blended samples under different curing time were inves-
Accepted 27 March 2019
tigated to explore the pozzolanic reaction of CBP. The results showed that the compressive strength of
Available online 12 April 2019
mortars contained CBP decreased gradually with the replacement level of CBP increasing at early age.
However, the compressive strength of blended mortars developed gradually at later curing time and
Keywords:
the mortar contained 20% achieved the highest compressive strength of 62.2 MPa at 90 days. The XRD
Recycled clay brick powder
Pozzolanic reaction
results demonstrated that the addition of CBP resulted in the formation of C-A-H gel in blended pastes
Compressive strength after 28 days. SEM pictures also found that the microstructure of blended pastes became more compact
Hydration product with curing time increasing, and SEM-EDS demonstrated that C-A-S-H gel was produced in blended
Microstructure pastes. Finally, it could be concluded that C-A-H and C-A-S-H gel were produced due to the pozzolanic
reaction of CBP and the microstructure of specimens with CBP became more compact, which lead to com-
pressive strength of blended specimens increasing gradually.
Ó 2019 Elsevier Ltd. All rights reserved.

1. Introduction by the European ceramic industry was typically 3–7% by weight of

red clay brick total production, suggesting that millions of clay
With the speeding up of urban construction and improvement, brick wastes were generated in Span. Nowadays the amount of clay
a large amount of solid wastes produced from the demolition of old brick waste is increasing shapely but its utilization ratio is very
buildings, has been produced in China. According to statistics [1,2], slow. It is widely reported that sintered clay brick, after commin-
the amount of solid wastes increased rapidly before 2013, then it uted, can be used as a pozzolanic material, which is rich in poz-
remained a high value about 3.26 billion tones, clay brick wastes zolanic ingredients [4–6]. Therefore, clay brick powder (CBP) has
accounted for around 50% especially. Furthermore, the study con- been used as raw materials or supplementary cementitious mate-
ducted by Haili Cheng [3] revealed that in the past five decades, rials to produce blended cement or alkali-activated cement, which
at least 20 billion meters cubed of clay brick products had been could meet for some demands of engineering projects [7]. The poz-
produced in China, which would mostly be transformed into solid zolanic activity of CBP in concrete was studied by Heidari. A and
waste in the next five decades. Studies performed by Pacheco- Hasanpour. B [8], who found that the compressive strength of con-
Torgal and Jalali [4] also found that the amount of waste generated crete with 20% CBP was 39.9 MPa, and the strength was decreased
by 3.23% compared with the reference mortar at 90 days. Previ-
⇑ Corresponding author at: Southeast University, School of Materials Science and ously experiments [9–11] demonstrated that the compressive
Engineering, Nanjing 211189, China. strength of waste brick-blended cement pastes was related to the
E-mail address: jmgao@seu.edu.cn (J. Gao). reaction degree of CBP and high compressive strength of waste

https://doi.org/10.1016/j.conbuildmat.2019.03.307
0950-0618/Ó 2019 Elsevier Ltd. All rights reserved.
210 J. Shao et al. / Construction and Building Materials 213 (2019) 209–215

brick-blended cement pastes (contained 10 and 20% waste brick hematite, feldspar (K2Al2Si6O6), are found in minor quantities. The amount of amor-
phous phase measured by means of semi-quantitative Rietveld refinement with on
powder) were consistent with the high amount of C-A-H and C-
XRD pattern was 20.1% in CBP.
A-S-H in hydration products. The pozzolanic reaction of CBP in
blended cement specimens was characterized by the development
2.2. Preparation of paste and mortar samples
of mechanical property simply in the research conducted by Puer-
tas. F et al. [12]. These studies commonly focused on the pozzolanic The mix proportion of specimens was given in Table 2. The water: binder (w/b)
reaction of CBP at early age, but the amount of CH produced by ratio was kept constant at 0.45 and the binder: sand (b/s) ratio was kept constant at
1:3. The cement was partially replaced by 0%, 10%, 20%, 30% and 40% of CBP by
cement hydration was not enough to react with active SiO2 and
weight. Each specimen was assigned a code e.g. B20 represented 20% replacement
Al2O3 at early ages and CBP mostly played the role of filling effect. of cement by CBP. The paste specimens were prepared in a Hobart mixer with a
Hence those studies might not be to put forward a further perspec- mixing time of two minutes, then were modelled in rectangular moulds
tive of the role of brick powder in hydration process. (40 mm  40 mm  160 mm) in their fresh states, which were kept under ambient
This paper primarily aims to explore the pozzolanic reaction of conditions (20 ± 1 ,with relative humidity >95%) for 24 h before being de-moulded.
The demoulded specimens were taken to curing room (at 20 ± 1 °C, 95% RH) until
CBP in blended cement mortars and pastes after 28 days. The effect
the certain test age (3, 7, 28, 60, and 90 days). The hydration reactions were stopped
of pozzolanic reaction on the mechanical property, hydration pro- with absolute alcohol. The mortars were cast into prismatic molds with the dimen-
duct, microstructure of blended cement pastes and mortars were sions of 40 mm  40 mm  160 mm and demoulded after 24 h. The curing condi-
researched systematically. It will provide a scientific evidence for tion of mortar was similar to that of pastes.
the application of CBP as supplementary cementitious material in
practical engineering. 2.3. Sample testing

The compressive strength was determined on the mortars according to Chinese

2. Materials and methodology Standard GB/T17671. Mineralogical phases of pastes were identified by X-ray
diffraction (XRD) at the step of 0.02°/min. The microstructure analysis was exam-
2.1. Materials ined on paste samples using Scanning electron microscopy (SEM). And Fourier
transform infrared spectroscopy (FTIR) was conducted to study the transformation
Recycled clay brick particles were milled with a laboratory mill to obtain the of mineral phase in the paste using the IR-100 spectrometer in transmittance mode
CBP. The particle size distribution of milled red clay brick was determined by a laser with a frequency range between 4000 and 400 cm 1. The samples were evaluated
diffraction particle size analyzer (Microtrac S3500, Microtrac, America). As shown using the compressed KBr pellet methodology.
in Fig. 1, the particle size of CBP ranged from 0.1 to 100 lm and the value of d50
was 15.89 lm. The pozzolanic activity of CBP was carried out based on Chinese
standard GB/T1596-2017 [13] and the measured value was 73.2%. Cement I 52.5 3. Results and discussion
(GB175) was adopted in this study. It is clearly that cement and CBP present a sim-
ilar particle distribution. The value of d50 of cement is 15.29 lm. The specific sur- 3.1. Compressive strength
face was measured by in accordance with Chinese standard GB/T8074-2008 [14],
and the measured value of CBP and cement were 360.5 m2/kg and 375.5 m2/kg,
respectively. The sand used in the mortars is river sand with 2.8 modulus. The influence of the content of CBP on the compressive strength
The chemical composition of clay brick powder and cement were analyzed by of blended mortars is shown in Fig. 3. Generally, the trend that the
the X-ray fluorescence analysis (XRF). As shown in Table 1, CBP is rich in SiO2 compressive strength of mortars increased with curing time
and Al2O3.
increasing was similar for all the samples. The strength values
The mineralogical composition of CBP was determined by X-ray diffraction
(XRD) from 5° to 70° (2h). As shown in Fig. 2, the major crystalline phase of CBP
for the control mortar at 3, 7, 28, 60 and 90 days were 25.7, 45.6,
is quartz and other compounds in the mineralogy of ceramic materials, such as

Q
Q: Quartz
100 F: Feldspar
90 H: Hematite
Brick powder
80 Cement

70

60
Cumu/%

50 Q
40

30

20 Q
QQ Q
10 FH F HH Q Q Q
Q
Q
Q
0
0.1 1 10 100 1000
5 10 15 20 25 30 35 40 45 50 55 60 65 70
Size(um)
2
Fig. 1. Cumulative particle size distribution of grounded clay brick powder and
cement. Fig. 2. X-ray diffraction patterns of CBP.

Table 1
chemical compositions (by mass %) of raw materials.

Compositions SiO2 Al2O3 Fe2O3 CaO K2O MgO SO3

CBP 63.6 18.6 9.11 1.65 1.82 1.28 0.02
Cement 19.96 4.44 3.05 61.80 0.76 1.85 3.06
 J. Shao et al. / Construction and Building Materials 213 (2019) 209–215 211

Table 2 of compressive strength of blended mortars after 28 days. J. M.

Mix proportion of specimens. Ortega et al. [18] also demonstrated that the development of com-
Sample codes Water/g Sand/g Binder/g pressive strength was due to more refined pore network produced
Cement Brick powder by both the pozzolanic activity and the effect of brick powder in
blended pastes.
B0 202.5 1350 450 0
B10 202.5 1350 405 45
B20 202.5 1350 360 90 3.2. X-ray diffraction analysis
B30 202.5 1350 315 135
B40 202.5 1350 270 180
Fig. 4 shows XRD patterns of the control paste at 3, 7, 28, 60 and
90 days, respectively. As shown in the picture, the diffraction peak
of calcium hydroxide could be identified at 18.15°, 28.82°, 34.25°,
3d 47.28°, 50.96°, and 54.52°. The band around 29°–32° corresponded
70 7d to the main peak of C3S and partial peak was belonged to C2S. With
28d
60d curing time increased, unreacted C3S particles hydrated continu-
60 ally, and the corresponding diffraction peak disappeared gradually.
Compressive strength /MPa

90d
Then the XRD curve was mainly consisted of the diffraction peak of
50 CH at 90 days. It is well known that CH consumption in pastes con-
tained pozzolanic material is related to the degree of pozzolanic
40 reaction. Therefore the degree of pozzolanic reaction is measured
by comparing the peak intensity and quantity of CH in blended
30 pastes with that of the reference mortar qualitatively.
As shown in Fig. 5, the diffraction peak of quartz appeared in the
20 diffraction curve of B20 sample. And characteristic peak of SiO2
were identified at 21.0°, 26.79° and 50.24°, respectively. Different
10
reaction product C-A-H gel was generated in B20 paste and the
characteristic peak was located at 8.5°. Kae-Long Lin et al [9] also
found that the C-A-H gel was generated in the cement paste con-
0
B0 B10 B20 B30 B40 taining brick power by XRD analysis. The intensity of characteristic
peak located at 18.15° increased gradually within 60 days, but it
Fig. 3. Compressive strength of blended mortars at different curing time. decreased from 60 days to 90 days. The amount of CH consumed
by the pozzolanic reaction exceeded that produced by cement
hydration from 60 days to 90 days, resulting in the loss of intensity
54.0, 57.7, and 59.6 MPa, respectively. The strength of B10, B20,
of diffraction peak at 18.15°. It was also consistent with the conclu-
B30 and B40 were decreased by 3.89%, 6.11%, 23.26% and 32.28%
sion that the pozzolanic reaction of CBP mainly occured from
compared with the reference mortar at 28 days, respectively. This
60 days to 90 days. Chindaprasirt. P et al. [19] also concluded that
behavior was agreed with the results discussed by Heidari. A
the degree of pozzolanic reaction in blended cement containing fly
et al. [8], who found that the compressive strength of mortars
ash was related to the intensity peak of CH and the intensity
decreased with the content of CBP increase, especially at early
decreased obviously at 90 days.
ages. However, the strength of blended mortars developed gradu-
From the results of Fig. 6, the intensity peak of SiO2 increased
ally at later curing time. And the compressive strength of B20 spec-
with the amount of CBP increase. Compared with the pattern of
imen reached the maximum value 62.2 MPa among all samples at
B20 paste, the new characteristic peak of SiO2 appeared at 36.70°
90 days, which indicated that the pozzolanic reaction of CBP lead
and 50.17° in B40 sample. It was also noticeable that the intensity
to the development of compressive strength of blended mortars
peak of CH decreased significantly with the increase of CBP content
[15]. This was probably that more active SiO2 and Al2O3 in CBP
and the intensity peak of C-A-H gel was stronger than that of B20
reacted with CH after 28 days and correspondingly more C-A-H
paste. The amount of cement in mixture decreased with the addi-
and C-A-S-H gel were produced, which could bind other hydration
products together. Other studies [9,16,17] also determined that the
degree of pozzolanic reaction increased gradually with the increase
of curing time, which could result in the compressive strength of —CH
mortars containing CBP approaching to that of the reference mor- —C3S
tar. Although the compressive strength of B30 and B40 mortars 90d
developed gradually with the curing time increase, they still did
not exceed to that of the reference mortar. This reason was that
the content of cement in the system reduced relatively with the 60d
large addition of CBP, which lead to the amount of C-S-H gel and
CH reducing. As a result, there was not enough CH to react with 28d
CBP to improve mechanical strength.
The relative content of cement decreased due to the incorpora-
tion of CBP, which led to the amount of hydration products 7d
decrease correspondingly, and the degree of cement hydration
was still low at early ages. Thus the filling effect of CBP contributed
3d
to partial compressive strength of blended mortars in initial stage.
With the hydration of cement continuous, the amount of hydration 10 20 30 40 50 60 70
products increased gradually resulting the filling effect of CBP
weakening. However, an additional hydration products produced
by the pozzolanic reaction of CBP was benefit for the development Fig. 4. XRD diffraction pattern of the control paste at 3, 7, 28, 60 and 90 days.
212 J. Shao et al. / Construction and Building Materials 213 (2019) 209–215

—SiO2 B40 764

2919 640
—CH 1658
—C3S 14621422 874
90d 3644
—C-A-H 3439
B20 970 460

2919 1658 764

60d
14621422 640

28d 3644 3439 874

B0 970 460
7d 1657
2919
14701428 456
3d 876
3644 3431 977
10 20 30 40 50 60 70
3500 3000 2500 2000 1500 1000 500

Wavenumber/cm-1
Fig. 5. XRD diffraction pattern of B20 paste at 3, 7, 28, 60 and 90 days.
Fig. 7. FTIR spectra of the cement paste with different content of CBP at 7 days.

Table 3
—CH FTIR of cement pastes containing clay brick powder.
—SiO2
Materials Characteristic vibrations Wave number Refer
90d —C-A-H
(cm 1)
—C3S
Ca(OH)2 –OH stretching vibration 3640 [21]
60d H2O m1 and m2 vibration 3440, 1658 [22]
CaCO3 C-O stretching vibration 1470–1422 [23]
C-S-H Si-O stretching vibration 970 [24]
28d
CaCO3 m3 out of plane vibration of CO23 874 [23]
SiO2 Si-O-Si symmetrical stretching vibration 764 [25]
C3S Out of plane bending (m4 O-Si-O) 640 [25]
asymmetric stretching vibration of Al-O 460
7d

3d owning to a decrease in the amount of CH produced in the cement

hydration.Table 4.
10 20 30 40 50 60 70
The FTIR spectra of B0, B20 and B40 pastes at 28 days are shown
in Fig. 8. The band located at 977 cm 1 was related to the stretch-
Fig. 6. XRD diffraction pattern of the B40 paste at 3, 7, 28, 60 and 90 days. ing vibration of Si-O in the C-S-H gel and the intensity of peak in B0
paste was the strongest among all samples at 28 days. This was in
accordance with the result of the compressive strength, which
tion of CBP, resulted in the decrease of hydration products. A com- mean that the degree of pozzolanic reaction was still low at
parison of patterns conducted by Altwair. N. M et al. [20] clearly 28 days.
showed that the intensity of CH peaks representing CH was signif- As shown in the Fig. 9, the intensity of absorption band at
icantly reduced with the increase in the content of pozzolan. 3644 cm 1 decreased sharply with the increase in the CBP content
and almost disappeared in the B40 sample at 90 days. Combined
3.3. FTIR analysis with the results of compressive strength, it determined that CH
produced by cement hydration was consumed to generate C-A-H
Fig. 7 presents the FTIR spectra of B0, B20 and B40 pastes at gel nearly in the B40 sample. At the same time, the degree of reac-
7 days. These spectra were basically similar and identical. It could
be seen that various bands shown in Table 3 were assigned corre-
spondingly. As shown in the figure, the absorption peak at Table 4
Microstructural analysis (EDS) of B20 and B40 pastes.
3640 cm 1 was belonged to O–H stretching vibration of CH. The
corresponding intensity peak of B20 paste was stronger than that Numbers Oxides/wt%
of B40 paste, which was consistent with the result of XRD analysis. SiO2 Al2O3 CaO
Owing to CBP addition, the absorption peak located at 764 cm 1
1 19.47 17.01 23.51
considering Si-O stretching vibration appeared in the infrared 2 19.47 11.34 25.05
spectrum. Clayden. N. J et al. [21] also determined that a series of 3 67.38 26.45 1.96
characteristic bands located at 1145, 1084, 769–758, 697 and 4 17.97 15.87 24.21
522 cm 1 were generated in the SiO2 spectrum. Furthermore, the 5 33.8 30.61 7.00
6 20.75 4.16 34.56
band associated with the unreacted C3S was also expected to
7 15.4 4.16 26.17
appear in B20 and B40 paste. The bands appeared between 8 47.06 1.13 6.44
1470 cm 1 and 1428 cm 1 in B0 paste were associated with the 9 36.58 5.4 16.37
C–O vibration in the CO23 , which originated from the reaction of 10 36.15 9.45 38.06
Cement 19.96 4.44 61.80
CH with CO2 in the atmosphere. The incorporation of brick powder
CBP 63.6 18.6 1.65
made corresponding absorption bands reduce the intensity,
 J. Shao et al. / Construction and Building Materials 213 (2019) 209–215 213

tion between CH and CO2 in the atmosphere decreased in the B40

B40
sample, which lead to corresponding band disappeared at
1462 cm 1. The absorption peak located at 764 cm 1 both disap-
2919 1658
640
peared almost in the B20 and B40 pastes at 90 days, corresponding
874 the most of active SiO2 in CBP dissolution. Studies performed by
1462 1422 764
B20 3644
3439 Trezza. M. A et al [22] also showed that a reduction of intensity
970 460
located at around 764 cm 1 was observed, which indicated that
1658
partial active SiO2 and Al2O3 had reacted in blended pastes. There-
2919
640 fore, active compositions in B20 and B40 samples had almost con-
1462 1422 764 sumed at 90 days and this conclusion was consistent with the XRD
B0 3644 3439 874 460
970 analysis.
1657
2919
1470 1428
3431
3.4. SEM analysis
876 456
3644 977

3500 3000 2500 2000 1500 1000 500 Investigations of hardened pastes were conducted by SEM at
-1 different curing times. Fig. 10 presents the microstructure of B0
Wavenumber/cm
paste at 7 days, 60 days and 90 days, relabeled as a, b, c respec-
Fig. 8. FTIR spectra of the cement paste with different content of CBP at 28 days. tively. As shown in Fig. 10(a), much fibrous C-S-H gel and some
crystalline CH were appeared at 7 days. With curing time increas-
ing, the microstructure of control paste became more compact,
B40 preventing micro-cracks formation and resulting in the structure
3644 1658 1422
970 640 460 more uniform.
3439
From the Fig. 11(a), a lot of CH with hexagon lamer shape can be
B20 found in B20 sample at 7 day. CH was consumed with CBP gradu-
1658
ally as curing time increased and the amount of CH was little in
2919
14621422 B20 paste at 90 days, which coincided with the resluts of B20 infra-
B0 3644 3439 874
970 460 red spetrum at 90 days. So it indirectly proved that the pozzolanic
1657
2919
reaction of CBP occurred mainly between 60d days and 90 days.
1470 1428
876
A significant phenomenon from the Fig. 12(a) was that the
456 amount of CH in B40 sample was less than that of B20 paste. Mean-
3644 3431 977
while, it was clear that a considerable amount of pores were
3500 3000 2500 2000 1500 1000 500 existed in B40 paste at 60 days. This was in accordance with the
Wavenumber/cm-1 conclusion of compressive strength analysis, which the strength
of B20 mortar exceed that of B40 at 60 days. Based on the above
Fig. 9. FTIR spectra of the cement paste with different content of CBP at 90 days. analysis, it was concluded that the addition of CBP could cause

Fig. 10. SEM images of the B0 paste at different curing times: (a) 7 days; (b) 60 days; (c) 90 days.

Fig. 11. SEM images of the B20 paste at different curing times: (a) 7 days; (b) 60 days; (c) 90 days.
214 J. Shao et al. / Construction and Building Materials 213 (2019) 209–215

Fig. 12. SEM images of B40 paste at different curing times: (a) 7 days; (b) 60 days; (c) 90 days.

Fig. 13. SEM images of B20 and B40 pastes at 90 days: (a) B20; (b) B40.

the microstructure of blended paste looser, and the size of micro- numbered 3, 5). The presence of these zones guaranteed the source
pores larger. As the pozzolanic reaction continued, CH was contin- of active SiO2 and Al2O3 in CBP to react with CH, correspondingly
ually consumed to produce new gel to fill in micropores that made forming C-A-S-H gel (points 1, 2, and 4). Kae-Long Lin et al. [9] also
blended pastes compact at 90 days. Mehmet S. Kirgiz [26] also found that the addition of CBP resulted in the formation of C-A-S-H
found that cement matrix containing 20 wt% CBP at 90 days had gel in the cement hydration product. The point 8 represent almost
denser microstructure than that of the mixture at 28 days. pure C-S-H gel. The analysis showed partial CBP were surrounded
by C-S-H gel produced by cement hydration and the Ca2+ invaded
3.5. EDS analysis into clay brick particles to form the C-A-S-H (points numbered 6,
7, 9 and 10). The location of each of these points were shown in
The microstructure of B20 and B40 pastes at 90 days was eval- the CaO-SiO2-Al2O3 ternary diagram Fig. 14.
uated by SEM-EDS. Fig. 13(a) shows partial hydrated CBP particles
combined the CaO-SiO2-Al2O3 ternary diagram analysis (points
4. Conclusions
Al2O3
0 The compressive strength, hydration products, microstructure
100
and energy spectrum of blended pastes and mortars prepared from
cement and CBP were investigated to explore the pozzolanic reac-
tion of CBP at different curing time in this study. From experimen-
25 tal results and discussions above, the following conclusions are
75
made:

(1) When the replacement level of CBP was no more than 20%,
50
50 the compressive strength of blended mortars was higher
5 than that of B0, and B20 mortar achieved the highest com-
pressive strength of 62.2 MPa at 90 days. When the amount
75 4 1 3 of CBP was more than 20%, the compressive strength of
25
2 blended mortars was less than that of B0, and the strength
CBP
increased with curing time increase.
Cement 7 10 9
(2) Hydration products of blended pastes not only contained CH
6
100 8 and C-S-H gel produced by cement hydration, but also C-A-H
0
CaO 0 25 50 75 100 SiO and C-A-S-H gel produced by the pozzolanic reaction.
2
(3) The pozzolanic reaction of CBP mainly occurred from
Fig. 14. Ternary diagram CaO-SiO2-Al2O3 of points marked in the B20 and B40 60 days to 90 days and the microstructure of blended pastes
micrograms. became compact.
 J. Shao et al. / Construction and Building Materials 213 (2019) 209–215 215

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Acknowledgements [14] GB/T8074-2008, Testing method for specific surface of cement-Blaine method.
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