Professional Documents
Culture Documents
https://doi.org/10.1007/s12517-020-05954-y
GMGDA 2019
Abstract
Aiming at the economic and environmental protection of fly-ash-metakaolin-based polymer concrete, the frost resistance of fly-
ash-metakaolin-based polymer concrete is studied. Concrete polymers were prepared by mixing 1:1 mass ratio fly ash with
metakaolin and using potassium silicate excitation. According to the content of fly ash and metakaolin, water-binder ratio, sand
ratio, and bone cement ratio, the soil-cement concrete blocks were divided into 7 groups. The effects of saturation volume
absorption of vacuum water, mass loss of freeze-thaw cycle, and relative dynamic elastic modulus on the frost resistance of
concrete specimens were tested. The results show that after curing for 3 days and 7 days, the compressive strength of soil polymer
concrete increases by 93.7% and 134.4% respectively. The increase of metakaolin content of fly ash can effectively improve the
structural compactness of soil-polymer concrete. When the water-cement ratio is 0.4%, the sand ratio is 0.25–0.30%, and the
bone cement ratio is 3.5%, the compressive strength and splitting tensile strength of geopolymer concrete are better. The
incorporation of fly ash and metakaolin can effectively reduce the vacuum saturation volume absorption rate and the freezing-
thawing water content of geopolymer concrete.
concrete (Xiao et al. 2017; Pranita et al. 2010). It was found Table 1 Main chemical constituents of fly ash and metakaolin (%)
that the addition of silica fume and metakaolin could effec- Main chemical constituents Fly ash Metakaolin
tively improve the freeze-thaw resistance of concrete. Xue
et al. (2017) carried out the freeze-thaw resistance test of con- SiO2 51.35 45.3
crete mixed with polyacrylonitrile fibers and metakaolin. It Al2O3 44.24 41.2
was found that the freeze-thaw resistance of concrete could CaO 0.13 3.77
be greatly improved by adding polyacrylonitrile fibers and Fe2O3 0.98 3.18
metakaolin. He et al. (2017) studied the fractal characteristics TiO2 0.9 1.62
of strength and microstructure of low water-binder ratio SO3 0 0.75
metakaolin concrete, and found that metakaolin could effec- MgO 0.48 0.44
tively improve the mechanical properties of concrete K2O 0.08 0.38
(Ghoddousi and Saadabadi 2017). P2O5 0.45 0.36
According to the current domestic research situation, most SrO 0 0.11
of the experiments are concentrated on the single-doped Na2O 0.16 0.09
metakaolin, and the study on the mixing of metakaolin and ZrO2 0 0.08
other mineral admixtures is less. Based on this, the mechanics MnO 0.01 0.05
and frost resistance of fly ash–metakaolin geopolymer con- Burning loss 0.72 2.4
crete are studied, and the influence of fly ash on the mechanics
of alkali-activated metakaolin geopolymer concrete is ex-
plored. The frost resistance of geopolymer concrete is im-
proved by using fly ash in order to provide support for the
development of geopolymer materials. compressive and splitting strength tests of geopolymer soil
concrete are carried out (Mishra and Behera 2010). Three
water-binder ratios (0.35, 0.4, 0.45), three sand ratios (0.25,
Materials and methods 0.30, 0.35), and three bone-binder ratios (3, 3.5, 4) are used to
prepare geopolymer soil concrete. Table 2 gives the grouping
Materials of geopolymer soil concrete specimens and their formulations.
Among them, GC-1-GC-7 is the grouping of geopolymer soil
The raw materials for preparing fly-ash-metakaolin-based concrete specimens (6 specimens in each group).
geopolymer concrete include the following (Li and Zhang Water-binder ratio = mass of water glass solvent/(mass of
2016): low calcium fly ash (secondary ash, taken from water glass solute + mass of fly ash + mass of metakaolin);
Guangzhou Huangpu Power Plant); metakaolin (taken from sand ratio = mass of sand/(mass of sand + mass of stone);
Shanxi Jinkun Heng Industry Co., Ltd., and the calcination bone-binder ratio = (mass of sand + mass of stone)/(mass of
temperature is 900 °C); industrial potassium silicate solution water glass solute + mass of fly ash + mass of metakaolin).
(modulus is 2.4, the concentration is 40%), flake potassium
hydroxide (purity ≥ 95%) and local river sand (after screening,
particle size is less than 2 mm), gravel (after cleaning and
screening, particle size is 5–20 mm). The main chemical com- 100
position and particle size distribution of low calcium fly ash
Passing size cumulative volume/%
90
and metakaolin are shown in Table 1 and Fig. 1.
As can be seen from Fig. 1, the particle size distribution of 80 Metakaolin
metakaolin is narrow (0.1–27.5 μm) and small (d50 = 4.8 μm). 70 Fly ash
40
Mix ratio of geopolymer soil concrete
30
potassium silicate solution) (Ni et al. 2016). Firstly, the Fig. 1 Diameter distribution curves of metakaolin and fly ash
Arab J Geosci (2020) 13:963 Page 3 of 10 963
Fly ash (kg/m3) 186 197 177 186 186 169 207
Metakaolin (kg/m3) 186 197 177 186 186 169 207
Potassium sodium silicate (kg/m3) 219 193 244 219 219 199 244
KOH (kg/m3) 61 54 68 61 61 55 68
Water (kg/m3) 63 56 70 63 63 57 70
Sand (kg/m3) 535 540 527 446 624 555 511
Gravel (kg/m3) 1249 1262 1236 1338 1160 1295 1192
Water-binder ratio/% 0.4 0.35 0.45 0.4 0.4 0.4 0.4
Sand rate/% 0.3 0.3 0.3 0.25 0.35 0.3 0.3
Bone glue ratio/% 3.5 3.5 3.5 3.5 3.5 4 3
Compressive strength/Mpa 56 32 35 54 36 32 43
Test block making and maintenance tested (Zou and Wu 2017; Leng et al. 2015). Compressive
strength test is carried out on electro-hydraulic servo pressure
The cubic geopolymer soil concrete block with 150-mm edge testing machine controlled by YAW-3000 micro-computer,
length is used in the test. The solid powder of fly ash, and splitting tensile strength test is carried out on electro-
metakaolin, and potassium sodium silicate solution are firstly hydraulic servo universal testing machine with WA-B screen
poured into the mixer for about 20 s; then, sand and stone are display. In the process of compressive strength test, continu-
poured into the mixer for about 140 s. After mixing, the ous uniform loading is adopted. According to the prediction of
geopolymer concrete is poured into the plastic mold, and then, the compressive strength of the test block, the loading speed of
the concrete is vibrated and compacted with the vibrating rod. 0.6 MPa/s is adopted in the compressive strength test. The
Finally, the surface is smoothed; that is to say, the geopolymer loading speed of splitting tensile strength test is 1/10 of that
concrete specimen is made. The data of this paper is obtained of compressive strength test.
from Earth data by NASA database (http://www.360doc.com/
content/19/0510/07/48503472_ 834712717.shtml). Test method for frost resistance
The setting and hardening speed of geopolymer soil con-
crete is fast, and it can reach a higher strength in a shorter time Testing of vacuum saturated volume absorption rate
(Zarauskas et al. 2017). Therefore, the specimens are watered of geopolymer soil concrete
and maintained in natural environment for 7 days, and the
mechanical properties of the specimens are tested after they The freeze-thaw cycle system adopted in the test of vacu-
are stationary indoors for 1 day including compressive and um saturated volume liquid absorption rate of geopolymer
splitting tensile strength tests. soil concrete is to freeze for 12 h in a low temperature box
at − 20 °C, then thaw for 12 h at 20 °C. After each freeze-
Mechanics test method thaw cycle, the unit area spalling amount of geopolymer
soil concrete is tested. When the cumulative amount ex-
Testing of composition and structure of geopolymer soil The ceeds 1.0 kg/m2, it is considered that the geopolymer soil
geopolymer is maintained for 7 days and is kept indoors for 1 concrete can reach the freeze-resistant limit (Wu et al.
day, then reserved after sampling and drying. The pore struc- 2018). The standard cured geopolymer soil concrete spec-
ture of the hardened body is tested by GT-60 mercury intru- imens are dried to constant weight m0, cooled to room
sion tester (driving pressure: 0.1-224.5 MPa) (Nili et al. 2016). temperature and saturated for 24 h in a vacuum saturator
The phase composition of the sample is analyzed by ARL with a vacuum of 6.7 kPa. The specimens are taken out and
XTRA X-ray diffractometer (Cu-Kα ray, angle: 5-80°, scan- the surface water is erased. The mass mΦ of the specimens
ning speed: 4°/min). The micro-morphology of the sample is is tested. Then, the volume V0 of the specimens is mea-
observed and analyzed by Quanta 200 environmental scan- sured by drainage method and the vacuum saturated vol-
ning electron microscope (accelerating voltage: 15 kV). ume liquid absorption rate of geopolymer soil concrete is
According to the Standard for Testing Methods of determined according to the vacuum saturated volume. The
Mechanical Properties of Ordinary Concrete, the mechanical following formula is calculated:
properties of geopolymer soil concrete at room temperature
ρ ¼ ðmΦ −m0 Þ=V 0 ð1Þ
are tested, and its compressive and splitting tensile strength are
963 Page 4 of 10 Arab J Geosci (2020) 13:963
Mass loss analysis of geopolymer soil concrete in freeze-thaw ash content on the compressive strength of geopolymer is
cycle shown in Fig, 2.
From Fig. 2, it can be seen that the compressive strength of
During the freeze-thaw cycle of geopolymer soil concrete, geopolymer soil at different curing ages increases gradually
mass loss records are made every 100 times (Wang and with the increase of fly ash content, and the extension of curing
Zhang 2017). When the mass loss rate exceeds 5%, it is con- age is beneficial to the improvement of the compressive
sidered that the geopolymer soil concrete specimens have strength of geopolymer. The compressive strength of
been destroyed (Sarsembayeva and Collins 2017). The mass geopolymer soil concrete specimen group (gc-6) with the low-
loss rate of geopolymer soil concrete specimens is calculated est content of metakaolin and fly ash is 25.5 Mpa and 29 mpa
according to formula (2): respectively on the 3rd and 7th day of curing period. When the
content of metakaolin and fly ash increases gradually, the com-
1 3 m0i −mni
ηn ¼ ∑ ð2Þ pressive strength of geopolymer concrete also increases gradu-
3 i¼1 m0i ally. The compressive strength of geopolymer soil concrete
specimen group (gc-7) with the highest content of metakaolin
In the formula, ηn is the mass loss rate (%) of geopolymer
and fly ash is 46.6 MPa and 68 MPa respectively on the 3rd and
soil concrete specimens after n freeze-thaw cycles, m0i is the
7th day of curing period. Compared with gc-6 group, the com-
mass (g) of the ith geopolymer soil concrete specimens before
pressive strength of the third and seventh day of the curing
freeze-thaw cycles, and m ni is the mass (g) of the ith
period increased by 93.7% and 134.4% respectively. It can be
geopolymer soil concrete specimens after n freeze-thaw cycles.
seen that under the same alkali excitation condition, fly ash and
metakaolin–based geopolymer soils are mixed into concrete,
Analysis of relative dynamic elastic modulus of geopolymer and the alkali excitation products are beneficial to the improve-
soil concrete under freeze-thaw cycle ment of compressive strength of concrete.
25.5
20
Results
10 µm 10 µm 10 µm
10 µm 10 µm
products are distributed in sheet structure, and some areas It can be seen from Fig. 4 that when the sand content
have holes. Increasing the content of fly ash and metakaolin increases from 0.25% to 0.30%, the compressive strength
is conducive to improving the structure compactness of of polymer concrete changes from 66% to 60%, reducing
geopolymer soil. When the content of fly ash and metakaolin by 6%. When the sand content continues to increase to
is relatively high ((Fig. 3c, Fig. 3 (d), and graph 3 (E)), a large 0.35%, the compressive strength of polymer concrete is
number of fly ash microbeads are wrapped in geopolymer gel, 40%, reduced by 20%, and the compressive strength is
and the different sizes of pores are peeling off mainly due to obviously reduced. When the sand content increases from
the fly ash microbeads. However, it can be seen from 0.25% to 0.30%, the splitting tensile strength will increase
geopolymer gel phase that the geopolymer gel phase formed from 50% to 55%. When the sand content continues to
after the excitation of large amount of fly ash and metakaolin increase, the splitting tensile strength will decrease.
is more compact, which accords with the analysis results of According to the results of compressive strength and split-
previous compressive strength tests. ting tensile strength, the optimal sand ratio is between
0.25 and 0.30%.
Compressive strength
Relationship between compressive strength and splitting
Splitting tensile strength
70 5.0 tensile strength at normal temperature
Compressive strength
Splitting tensile strength
70 4.0
Splitting tensile strength/MPa
3.5
Splitting tensile strength/Mpa
Compressive strength/MPa
50 3.0 3
2.0 2.5
30
2
10 1.0 10 20 60 40 50 60 70
0.35 0.40 0.50 compressive strength/MPa
Water-binder ratio/% Fig. 7 Relationship between compressive strength and splitting tensile
Fig. 6 Effect of water-cement ratio on compressive and splitting strength strength of geopolymer soil concrete at room temperature
Arab J Geosci (2020) 13:963 Page 7 of 10 963
Table 3 Vacuum saturated volume absorption rate of geopolymer soil From Table 4, it can be seen that when the content of
concrete
metakaolin and fly ash is high, with the increase of freeze-
Group Vacuum saturated volume absorption rate/% thaw cycles, the mass loss of the samples of GC-3 groups
firstly appears negative value. This is because with the in-
GC-1 13.1 crease of freeze-thaw cycles, the number and volume of
GC-2 12.5 micro-cracks in the concrete of geopolymer soil increase, the
GC-3 14.9 cracks absorb water or the hydration reaction occurs, etc. at
GC-4 13.2 the initial stage of freeze-thaw, resulting in that water absorp-
GC-5 13.3 tion is greater than surface peeling, leading to increased mass
GC-6 15.4 (Kumar et al. 2010). When the number of freeze-thaw cycles
GC-7 11.6 reaches 1200, the mass loss rate of all geopolymer concrete
specimens is less than 5%. This shows that the geopolymer
concrete specimens have not frozen out, and their frost resis-
geopolymer soil can form a more compact concrete structure, tance grade is above F1200, and the mass loss rate of
the vacuum saturated volume liquid absorption rate of the geopolymer soil concrete specimens with higher content of
geopolymer soil concrete specimens is tested. The results are metakaolin and fly ash is less than that of geopolymer soil
shown in Table 3. concrete specimens with lower content of both. When mixed
It can be seen from Table 3 that the vacuum water saturated with fly ash, the frost resistance of geopolymer soil concrete
volume liquid absorption rate of geopolymer soil concrete is can be improved.
large, which is because the pores of geopolymer soil concrete
will form after a large amount of free water evaporates. The
mixing of fly ash and metakaolin in geopolymer concrete can Analysis of relative dynamic elastic modulus of geopolymer
effectively reduce the vacuum saturated volume absorption soil concrete under freeze-thaw cycle
rate of geopolymer concrete. The higher the content of fly
ash and metakaolin is, the lower the vacuum saturated volume The influence of freeze-thaw cycles on the relative dynamic
absorption rate is. Under the same conditions, the frozen water modulus elastic modulus of geopolymer soil concrete is
content of geopolymer concrete is lower and the frost resis- shown in Table 5.
tance of geopolymer concrete is improved. From Table 5, it can be seen that the relative dynamic
elastic modulus of geopolymer concrete specimens is more
than 80% after 1200 freeze-thaw cycles, which indicates that
Mass loss of geopolymer soil concrete in freeze-thaw cycle geopolymer concrete has not frozen out, and the relative dy-
namic elastic modulus of geopolymer concrete with higher
The mass loss of geopolymer soil concrete during freeze-thaw content of metakaolin and fly ash is larger than that of
cycles is shown in Table 4. geopolymer concrete with lower content of metakaolin and
Number of freeze-thaw Mass loss rate in group Mass loss rate in group Mass loss rate in group Mass loss rate in group Mass loss rate in group
cycles GC-1/% GC-2/% GC-3/% GC-6/% GC-7/%
100 0 0 0 0 0
200 0 0 0 0 0
300 0 0 0 0 0
400 0 0 − 0.017 0 0
500 0 0 0.009 0.013 0
600 0.006 0 0.013 0.016 0
700 0.019 0 0.044 0.044 0
800 0.031 − 0.009 0.052 0.057 0.008
900 0.048 0.019 0.068 0.078 0.031
1000 0.057 0.031 0.077 0.082 0.039
1100 0.060 0.034 0.089 0.103 0.052
1200 0.092 0.057 0.126 0.133 0.068
963 Page 8 of 10 Arab J Geosci (2020) 13:963
Table 5 Analysis of the impact of freeze-thaw cycle on the relative dynamic elastic modulus of ground polymer soil concrete
Number of Relative dynamic elastic Relative dynamic elastic Relative dynamic elastic Relative dynamic elastic Relative dynamic elastic
freeze-thaw modulus of gc-1 group/% modulus of gc-2 group/% modulus of gc-3 group/% modulus of gc-6 group/% modulus of gc-7 group/%
cycles
100 0 0 0 0 0
200 99.5 99.7 99.4 99.4 99.7
300 99.0 99.5 99.1 98.9 99.5
400 98.2 99.2 98.3 98.1 99.2
500 97.7 98.6 97.8 97.6 98.5
600 97.7 98.2 97.2 97.2 97.7
700 96.5 97.4 96.4 95.6 96.9
800 95.0 96.9 94.1 93.4 96.4
900 93.1 96.2 92.3 91.9 95.7
1000 92.2 95.6 90.9 87.8 95.1
1100 90.0 94.3 88.2 86.3 93.0
1200 88.8 92.5 86.0 84.4 90.6
fly ash, showing that the mixing of metakaolin and fly ash can emission from coal-fired power plants is increasing year by
improve the frost resistance of the concrete. year, and it has become one of the industrial waste residues
In order to verify the frost resistance of concrete with dif- with large discharge in China. A large number of fly ash
ferent compositions, the frost cracking of concrete is com- without treatment will produce dust and pollute the atmo-
pared at different temperatures. The results are shown in sphere; if discharged into the water system, it will cause river
Table 6. siltation and toxic chemicals will also cause harm to human
It can be seen from Table 6 that for the concrete at different and biological. The small particle size of fly ash (400–600
temperatures, there are differences in the frost cracking of mesh) can play a role of compact filling and improve the
concrete. When the temperature is – 10 °0, there is no frost compactness and uniformity of concrete. Fly ash contains high
crack in GC-1 and GC-3. The frost cracking degree of GC-2 amorphous silica-aluminum structure, most of which are used
and GC-4 concrete is 12%, that of gc-5 is 8%, that of gc-6 is as cementitious materials to partly or completely replace ce-
11%, and that of gc-7 is 12%. Analysis of the overall data ment, and its characteristics become the preferred raw material
shows that the frost resistance of GC-3 group is the best. for the preparation of geopolymer concrete.
Conclusions He ZM, Zou JQ, Liu AH, Wang HY (2017) Effect of liquid-solid ratio
and maintenance mechanism on flow ability and mechanical prop-
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In this paper, the mechanics and frost resistance tests of fly- 98–101
ash-metakaolin-based aggregate concrete are carried out. Kulovaná T, Vejmelková E, Keppert M (2016) Mechanical, durability
Through the mechanical compressive strength, micro-mor- and hygrothermal properties of concrete produced using Portland
phology, splitting tensile strength, and frost resistance tests cement-ceramic powder blends. Struct Concr 17:105–115
Kumar S, Kumar M, Jagdish Ahmad I (2010) Investigation into the char-
of geopolymer concrete, the following conclusions are drawn: acterization of fly ash collected from different thermal power sta-
tions of India. J Mines Met Fuels 58(6):162–167
(1) The compressive strength of fly ash–metakaolin soil Leng FG, Wang YM, Zhou YX, Gao C (2015) Discussion on existing
polymer concrete increases with the increase of the con- problems and suggestions for revision of GB/T50081-2002 standard
for testing methods of mechanical properties of ordinary concrete.
tent of fly ash and metakaolin. Under the condition of no The 6th National Special Concrete Technology (High Performance
admixture, when the water binder ratio is 0.4%, the sand Concrete Special) Exchange Conference, Yinchuan, China, pp.27-
ratio is 0.25–0.3%, and the bone glue ratio is 3.5%, 48
geopolymer earth concrete can obtain the best compres- Li WJ, Zhang Q (2016) Analysis of dynamic response for concrete wall
under blast load. Comput Simul 33:27–31
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Liu J, Liu Y, Wang X (2019) An environmental assessment model of
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geopolymer concrete with high content of metakaolin case study in Guangzhou. Environ Sci Pollut Res Int. https://doi.
and fly ash after 1200 freeze-thaw cycles are smaller than org/10.1007/s11356-019-07107-5
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Funding The study was supported by “Project of Special Fund for Basic ability to find suitability of fly ash and over burden materials for
Scientific Research Operating Expenses of Central Universities, China filling of voids in fire affected mine. J Mines Met Fuels 58(1-2):24–
(Grant No. 2572017BB05)”, and “the National Natural Science 26
Foundation of China (Grant No. 51708092)”. Ran K (2015) Impact of CaO content on mechanical performance of slag-
based geopolymer cement. J Guizhou Normal Univ(Nat Sci) 33(4):
96–99
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