Production of High Compressive Strength Geopolymers Considering Fly Ash or Slag Chemical Composition

Koumoto, Tatsuya

doi:10.1061/(ASCE)MT.1943-5533.0002788

Open access

Technical Notes

May 23, 2019

Production of High Compressive Strength Geopolymers Considering Fly Ash or Slag Chemical Composition

Author: Tatsuya Koumoto, Ph.D. https://orcid.org/0000-0001-6889-5072 [email protected]Author Affiliations

Publication: Journal of Materials in Civil Engineering

Volume 31, Issue 8

https://doi.org/10.1061/(ASCE)MT.1943-5533.0002788

PDF

Abstract

More than

60 billion kg

(

60 million t

) of industrial by-products such as fly ash, garbage melting furnace slag, and steel slag are generated every year in Japan. Almost all of them seem to have been effectively used in mixtures with cement according to their chemical and mechanical characteristics in the field of civil work. Fly ash and slags can be used to create geopolymers in a process that emits less carbon dioxide than does the cement-making process. This reduction in

{CO}_{2}

emission is important because

{CO}_{2}

is one of the substances known to contribute to global warming. In the future, further uses of these fly ash and slags must be explored. The chemical mechanism for hardening composite materials by mixing aluminosilicate binders such as fly ash and slags with alkaline activators such as liquid NaOH and sodium silicate is known as a geopolymeric reaction, and the hardened composite material is called geopolymer. Geopolymers are produced by mixing two components of solid binders, such as fly ash, slags, and so on, with liquid activators such as NaOH, KOH, sodium silicate, and so on. Geopolymers have recently been developed to be used as a replacement for portland cement concrete. Research has been done to improve the compressive strength characteristics of both geopolymers and the combination of soft soil and fly ash–based geopolymer. The development of high compressive strength geopolymer using fly ash and slags will strongly contribute to the fields of construction, geotechnical engineering, and architecture. This paper describes the method for production and strength diagnosis of geopolymers considering the chemical composition of fly ash or slags.

Introduction

In 1979, Davidovits discovered the chemical mechanism for hardening composite materials resulting from geopolymeric reactions by mixing aluminosilicate binders with alkaline activators (Davidovits 1991, 2013). Geopolymers have recently been developed to use as a replacement for portland cement concrete, the cement of which discharges 1,000 kg (1.0 t)

{CO}_{2}

to produce 1,000 kg (1 t) cement (Ikeda and Mikuni 2006). Although geopolymers typically outperform portland cement concrete in compressive strength, the high cost of the alkaline activator and underdeveloped quality assurance (QA) and quality control (QC) have been the primary barriers that have prevented geopolymers from being used in construction and other industries. Buchwald (2006) defined geopolymers as being produced by mixing two components: a solid binder, such as fly ash, slags, and so on; and a liquid activator, such as NaOH, KOH, sodium silicate, and so on.

According to many studies, factors affecting the compressive strength

q_{u}

include the chemical composition of solids; fineness of materials;

w

, the ratio of solution (NaOH + sodium silicate) to solid;

η

, the ratio of NaOH to sodium silicate; the curing time; the curing temperature; the molarity of NaOH (Suresh and Manojkumar 2013; Budh and Wahhade 2014); and so on. In addition to

w

and

η

, the composition of the fly ash and slags is another important variable.

This paper describes the method of production, strength diagnosis, and strength improvement of geopolymers made from binders of fly ash and slags, which are then mixed with activators (solutions of NaOH and sodium silicate). The chemical compositions of the binders are taken into account to find the optimum values of

w

and

η

which yields the maximum compressive strength

q_{u \max}

that is greater than

70 N / {mm}^{2}

(Pawan Kumar and Surendra 2016).

Materials

Preparation of Geopolymer Materials

Steelmaking slags and garbage melting furnace slags are provided as granular materials, unlike fly ash. The particle size

d_{50}

of materials seems to affect the compressive strength of geopolymers

q_{u}

(Fig. 1). The finer the particle size, the greater is the compressive strength of geopolymers. In the present tests, all slags were ground after being air dried to a maximum particle size of 0.106 mm for effective chemical reaction.

Fig. 1. Effect of slag particle size ( $d_{50}$ ) on compressive strength.

Chemical Compositions of Geopolymer Materials

The main chemical compositions of the geopolymer materials tested are listed in Table 1. The six kinds of geopolymer materials, two each of Fly ash, Slag 1 (steel factory slags), Slag 2 (garbage melting furnace slags), were the starting geopolymer materials, and ten mixtures of two each of fly ash and fly ash, fly ash and Slag 1, fly ash and Slag 2, and Slag 1 and Slag 2, were prepared as materials with a wide range of chemical compositions.

Table 1. Chemical composition of tested geopolymer materials

Geopolymer material	Geopolymer sample	Chemical composition (%)
Geopolymer material	Geopolymer sample	${SiO}_{2}$	${Al}_{2} O_{3}$	CaO	${Fe}_{2} O_{3}$	MgO	${SO}_{3}$
Fly ash	Reihoku	55.0	21.1	9.1	5.3	1.1	0.9
Fly ash	Karita	38.8	24.3	19.5	1.6	0.5	6.6
Slag 1	Koro	34.6	14.8	42.7	0.4	5.7	0.0
Slag 1	Stainless	26.7	5.3	48.2	1.0	5.5	0.4
Slag 2	Kazusa	34.2	13.2	42.0	2.6	1.9	0.7
Slag 2	Narashino	34.2	13.9	39.3	3.7	1.8	0.6
Fly ash and fly ash	KariRei	46.9	22.7	14.3	3.5	0.8	3.8
Fly ash and fly ash	KariRei2	49.6	22.2	12.6	4.1	0.9	2.8
Fly ash and Slag 1	ReiKoro	44.8	18.0	25.9	2.9	3.4	0.5
	ReiKoro2	41.4	16.9	31.5	2.0	4.2	0.3
	KariKoro	36.7	19.5	31.1	1.0	3.1	3.3
	KariKoro2	36.0	18.0	35.0	0.8	4.0	2.2
Fly ash and Slag 2	ReiKazu	44.6	17.2	25.6	4.0	1.5	0.8
Fly ash and Slag 2	ReiNara	44.6	17.5	24.2	4.5	1.4	0.8
Slag 1 and Slag 2	KazuKoro	34.4	14.0	42.4	1.5	3.8	0.4
Slag 1 and Slag 2	KazuKoro2	34.5	14.3	42.5	1.1	4.4	0.2

Note: Koro = ground blast furnace slag; Stainless = ground stainless steel–making slag. Mixture ratio of geopolymer samples: KariRei: $Karita ∶ Reihoku = 1 ∶ 1$ by weight; $KariRei 2 ∶ Karita$ : Reihoku = $1 ∶ 2$ by weight; ReiKoro: $Reihoku ∶ Koro = 1 ∶ 1$ by weight; ReiKoro2: $Reihoku ∶ Koro = 1 ∶ 2$ by weight; KariKoro: $Karita ∶ Koro = 1 ∶ 1$ by weight; KariKoro2: $Karita ∶ Koro = 1 ∶ 2$ by weight; ReiKazu: $Reihoku ∶ Kazusa = 1 ∶ 1$ by weight; Rebyara: $Reihoku ∶ Narashbyo = 1 ∶ 1$ by weight; KazuKoro: $Kazusa ∶ Koro = 1 ∶ 1$ by weight; and KazuKoro2: $Kazusa ∶ Koro = 1 ∶ 2$ by weight.

Making Geopolymer Samples

Although several kinds of liquid sodium hydroxide and sodium silicate are available as activators, for the purpose of this research 48% NaOH (

18 mol / L

) and sodium silicate (

{Na}_{2} \cdot n {SiO}_{2}

,

n = 3.2

) were chosen due to their commercial availability and high concentration, with the expectation to yield high compressive strength geopolymers. The compressive strength of geopolymers,

q_{u}

, is generally considered to be a function of the weight ratio of activator to binder,

w

, and the weight ratio of NaOH to sodium silicate,

η

. In this research, initially, geopolymer samples were made for wide range of ratios of

w

(0.3–0.6) and

η

(0.0–1.0), depending on geopolymer materials for fly ash, Slag1 and Slag2.

For mixtures of geopolymer materials, geopolymer samples were made for variable

η

values at a constant value of

w = 0.4

, according to the aforementioned compression test results. After mixing the activator and binder, the geopolymer samples were placed in plastic molds of diameter

D = 50

mm and height

H = 100

mm, and vibrated slightly. The geopolymer samples were removed from the molds after 1 or 2 days and cured at room temperature under dry condition for 28 days.

Tests and Results

Before compression tests, physical properties of geopolymer samples such as diameter

d

, height

h

, and weight

W

were measured to obtain characteristics of shrinkage and density.

Compression tests of geopolymer samples were carried out at the Saga Construction Technology Support Organization (SCTSO) using the concrete testing apparatus in the same test method for concrete samples (sample diameter

d = 50 mm

and height

h = 100 mm

, loading

rate = 0.6 \pm 0.4 N / {mm}^{2}

, and loading plate

φ = 300 mm

).

Compression test results are shown in Fig. 2 for key geopolymer samples and Fig. 3 for mixture geopolymer samples. Fig. 2 shows the relationship between the compressive strength

q_{u}

and

η

value for each

w

value. Fig. 3 shows the relationship between

q_{u}

and

η

only for

w = w_{opt} = 0.4

, which was determined from Fig. 2. Characteristics of the volume shrinkage ratio

Δ V / V

at

q_{u \max}

are summarized in Table 2.

Fig. 2. Compression test results for fly ash and slag geopolymers: (a) Reihoku; (b) Karita; (c) Koro; (d) Stainless; (e) Kazusa; and (f) Narashino.

Fig. 3. Compression test results for mixture materials geopolymers.

Table 2. Shrinkage characteristics of geopolymer samples at

q_{u \max}

Geopolymer sample	$q_{u \max}$ ( $N / {mm}^{2}$ )	$d$ (mm)	$Δ d$ (mm)	$h$ (mm)	$Δ h$ (mm)	$Δ V$ ( ${mm}^{3}$ )	$Δ V / V$ (%)
Reihoku	45.2	50.0	0.0	99.8	0.2	392.7	0.20
Karita	104.3	50.0	0.0	99.8	0.2	392.7	0.20
Koro	168.0	49.8	0.2	99.6	0.4	2,346.8	1.20
Stainless	48.1	48.1	1.9	95.8	4.2	22,270.9	11.34
Kazusa	110.0	49.7	0.3	99.7	0.3	2,931.1	1.49
Narashino	86.4	49.9	0.1	99.6	0.4	1,566.9	0.80
KariRei	70.1	49.9	0.1	99.6	0.4	1,566.9	0.80
KariRei2	40.9	49.8	0.2	99.8	0.2	1,957.2	1.00
ReiKoro	79.3	49.9	0.1	99.7	0.3	1,371.3	0.70
ReiKoro2	118.0	49.8	0.2	99.6	0.4	2,346.8	1.20
KariKoro	117.0	49.9	0.1	99.5	0.5	1,762.4	0.90
KariKoro2	159.0	49.9	0.1	99.7	0.3	1,371.3	0.70
ReiKazu	102.0	49.8	0.2	99.4	0.6	2,736.3	1.39
ReiNara	94.3	49.7	0.3	99.3	0.7	3,707.1	1.89
KazuKoro	132.0	49.8	0.2	99.5	0.5	2,541.6	1.29
KazuKoro2	166.0	49.8	0.2	99.3	0.7	2,931.1	1.49

Note: $d$ = diameter, $h$ height; $V$ = initial volume of geopolymer sample; $Δ d$ , $Δ h$ , and $Δ V$ = amount of shrinkage of $d$ , $h$ , and $V$ , respectively; and $Δ V / V$ = volume shrinkage ratio.

Discussions

Determination of $w_{opt}$ , $η_{opt}$ , and $q_{u \max}$

In Fig. 2

q_{u}

generally increases with a decrease in

η

for each

w

value and reach the maximum value

q_{u \max}

at a certain

η

value for the case of

w = 0.4

. The

w

value which yields the

q_{u \max}

is defined as the optimum value

w_{opt}

;

w_{opt}

is a constant of 0.4 for all key geopolymers.

Olivia and Nikraz (2012) and Prakash and Urmil (2012) evaluated how the ratio of alkaline liquid to fly ash affected the compressive strength of geopolymer. Olivia and Nikraz (2012) mentioned that the ratio,

w

, in the range 0.30–0.45 improved the strength to a certain extent, and Prakash and Urmil (2012) mentioned that the ratio,

w

, in the range of 0.30–0.40 did not much improve the strength. The values of

q_{u \max}

were produced at

w_{opt} = 0.4

, similarly to Olivia and Nikraz (2012) and Prakash and Urmil (2012).

The maximum value

q_{u \max}

occurs at a certain

η

value, which is defined as the optimum value

η_{opt}

(Fig. 2). From Fig. 3 which shows the relationship between

q_{u}

and

η

for mixture material geopolymer for a constant value of

w = w_{opt} = 0.4

, the values of both

q_{u \max}

and

η_{opt}

were obtained.

The values of

w_{opt}

,

η_{opt}

, and

q_{u \max}

from Fig. 2 and the values of

η_{opt}

and

q_{u \max}

from Fig. 3 are summarized in Table 3. Table 3 also includes the values of the density

ρ_{t}

of geopolymer samples at the

q_{u \max}

and the volume shrinkage ratio

Δ V / V

.

Table 3. Compression test results of geopolymer samples

Geopolymer materials	Geopolymer samples	Compression test results
Geopolymer materials	Geopolymer samples	$q_{u \max}$ ( $N / {mm}^{2}$ )	$w_{opt}$	$η_{opt}$	$ρ_{t}$ ( $kg / m^{3}$ )	$Δ V / V$ (%)
Fly ash	Reihoku	45.2	0.40	0.80	1,868	0.20
Fly ash	Karita	104.3	0.40	0.50	1,985	0.20
Slag 1	Koro	168.0	0.40	0.40	2,227	1.20
Slag 1	Stainless	48.1	0.40	0.00	2,269	11.34
Slag 2	Kazusa	110.0	0.40	0.30	2,202	1.49
Slag 2	Narashino	86.4	0.40	0.50	2,043	0.80
Fly ash and fly ash	KariRei	70.1	0.40	0.65	1,971	0.80
Fly ash and fly ash	KariRei2	40.9	0.40	0.70	1,986	1.00
Fly ash and Slag 1	ReiKoro	79.3	0.40	0.60	2,098	0.70
	ReiKoro2	118.0	0.40	0.60	2,144	1.20
	KariKoro	117.0	0.40	0.45	2,122	0.90
	KariKoro2	159.0	0.40	0.43	2,149	0.70
Fly ash and Slag 2	ReiKazu	102.0	0.40	0.55	2,081	1.39
Fly ash and Slag 2	ReiNara	94.3	0.40	0.65	2,024	1.89
Slag 1 and Slag 2	KazuKoro	132.0	0.40	0.35	2,219	1.29
Slag 1 and Slag 2	KazuKoro2	166.0	0.40	0.36	2,218	1.49

Note: $q_{u \max}$ = maximum value of compressive strength $q_{u}$ ; $w_{opt}$ = optimum value of $w$ yielding $q_{u \max}$ ; $η_{o p t}$ = optimum value of $η$ yielding $q_{u \max}$ ; $ρ_{t}$ = density of geopolymer sample at $q_{u \max}$ ; and $Δ V / V$ = volume shrinkage ratio of geopolymer sample.

Correlation between $η_{o p t}$ and Chemical Compositions of Binders

Because geopolymerization is a chemical reaction, specifically an aluminosilicate reaction, the amount of NaOH which contributes to ionize metals contained in the binder increases with the increase of the amount of

{Al}_{2} O_{3}

and

{SiO}_{2}

. Accordingly,

η

, which is the weight ratio of NaOH to sodium silicate, is considered as the function of

C_{a s} (= {Al}_{2} O_{3} + {SiO}_{2})

. Fig. 4 shows the correlation between

η_{opt}

and

C_{a s}

. The relationship between

η_{opt}

and

C_{a s}

is well correlated and expressed by the straight line with a high correlation coefficient of

r = 0.949

as

η_{opt} = 0.0157 C_{a s} - 0.414

(1)

Fig. 4. Correlation between $η_{opt}$ and $C_{a s}$ .

Eq. (1) is used to calculate the

η_{opt}

value from the value of

C_{a s}

of binders to effectively produce high compressive strength geopolymers.

Correlation between $q_{u \max}$ and Chemical Compositions of Binders

The value of

q_{u \max}

generally decreases with the increase of the amount of each

{SiO}_{2}

,

{Al}_{2} O_{3}

, and

{Fe}_{2} O_{3}

(Tables 1 and 3). In contrast,

q_{u \max}

is in proportion to the content of CaO. Because the total contents of chemical compositions are constant, binders which have high content of

{SiO}_{2}

or

{Al}_{2} O_{3}

are said to be binders which have less content of CaO. Using the factor of

CaO / C_{a s}

, the mutual chemical characteristics of

q_{u \max}

can be shown. Fig. 5 shows the relationship between

q_{umax}

and

CaO / C_{a s}

. Binders with

CaO / C_{a s}

in the range 0.3–0.9 yielded high compressive strength geopolymers with

q_{u \max}

=

80 - 168 N / {mm}^{2}

(Fig. 5).

Relationship between $q_{u \max}$ and $η_{opt}$

Fig. 6 shows the relationship between the

q_{u \max}

and

η_{opt}

. Test data obtained by Prakash and Urmil (2012) (

q_{u \max} = 40 N / {mm}^{2}

for

η_{opt} = 0.5

), Pawan Kumar and Surendra (2016) (

q_{u \max} = 70.6 N / {mm}^{2}

for

η_{opt} = 0.83

), and Mustafa Al Baki et al. (2012) (

q_{u \max} = 57 N / {mm}^{2}

for

η_{opt} = 0.4

) are plotted; they all lie in the lower range of the present

q_{u \max}

. Some reasons for their lower compressive strengths are the difference of the chemical compositions of binders, the value of

w

, curing conditions, and so on. In Fig. 6, the

q_{u \max}

becomes greater than

100 N / {mm}^{2}

for

η_{opt}

in the range 0.3–0.5.

Fig. 6. Relationship between $q_{u \max}$ and $η_{opt}$ .

Shrinkage of Geopolymer Samples

Fig. 7 shows the relationship between the volume shrinkage ratio of geopolymer samples

Δ V / V

and

CaO / C_{a s}

. The values of

Δ V / V

were generally less than 2%. These results will be helpful for the design of geopolymer construction.

Fig. 7. Relationship between $Δ V / V$ and $CaO / C_{as}$ .

Conclusions

The methods for production and strength diagnosis of geopolymers to determine the optimum values of

w_{opt}

and

η_{opt}

yielding the maximum compressive strength

q_{u \max}

, and to correlate

η_{opt}

with the appropriate chemical composition of binders to produce effectively the high compressive strength geopolymers, are as follows:

1.

to produce high compressive strength geopolymer, slags have to be ground as fine as possible;

2.

the value of

q_{u}

generally becomes the maximum value (

q_{u \max}

) when the weight ratio,

w

, of the mixed solutions of NaOH and sodium silicate to the binder is 0.4 (

w_{opt}

, which is the optimum value of

w

yielding

q_{u \max}

), regardless of the type of the binder;

3.

there is an optimum value,

η_{opt}

(the weight ratio of NaOH to sodium silicate), yielding

q_{u \max}

for each binder;

4.

the value of

η_{opt}

is well correlated with the factor

C_{a s}

[Eq. (1)];

5.

The value of

η_{opt}

for an arbitrary binder necessary to manufacture high compressive strength geopolymer is calculated by Eq. (1);

6.

binders with

CaO / C_{a s}

in the range 0.3–0.9 (

η_{opt} = 0.3 - 0.5

) yield high compressive strength geopolymers with

q_{u \max} = 80 - 168 N / {mm}^{2}

; and

7.

the volume shrinkage ratio

Δ V / V

is generally less than 2%.

Notation

The following symbols are used in this paper:

$C_{a s}$: ${Al}_{2} O_{3} + {SiO}_{2}$ (%);
$CaO / C_{a s}$: factor;
$D$: diameter of mold (mm);
$d$: diameter of geopolymer sample (mm);
$d_{50}$: particle size in 50% of particles by mass (mm);
$H$: height of mold (mm);
$h$: height of geopolymer sample (mm);
$q_{u}$: compressive strength ( $N / {mm}^{2}$ );
$q_{u \max}$: maximum compressive strength ( $N / {mm}^{2}$ );
$r$: correlation coefficient;
$V$: volume of mold ( ${mm}^{3}$ );
$w$: weight ratio of activator solution of sodium hydroxide + sodium silicate) to binder;
$w_{opt}$: optimum value of $w$ at yielding $q_{u \max}$ ;
$Δ V$: amount of shrinkage of geopolymer sample ( ${mm}^{3}$ );
$Δ V / V$: volume shrinkage ratio of geopolymer sample (%);
$η$: weight ratio of solution of sodium hydroxide to sodium silicate;
$η_{opt}$: optimum value of $η$ at yielding $q_{u \max}$ ; and
$ρ_{t}$: density of geopolymers at $q_{u \max}$ ( $kg / m^{3}$ ).

Acknowledgments

The author is grateful to Maruwa Giken for preparing ground solid waste incinerator slags. The author is also grateful to Kyuden Sangyo, Shunan Works, Nisshin-Steel, and Nippon Steel & Sumikin Slag Products for contributing coal-fired power plant ash, stainless manufactured slag, and ground granulated blast slag, respectively.

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Published In

Journal of Materials in Civil Engineering

Volume 31 • Issue 8 • August 2019

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This work is made available under the terms of the Creative Commons Attribution 4.0 International license, http://creativecommons.org/licenses/by/4.0/.

History

Received: Mar 10, 2018

Accepted: Feb 4, 2019

Published online: May 23, 2019

Published in print: Aug 1, 2019

Discussion open until: Oct 23, 2019

Authors

Affiliations

Tatsuya Koumoto, Ph.D. https://orcid.org/0000-0001-6889-5072 [email protected]

Professor Emeritus, Dept. of Agricultural Sciences, Saga Univ., 1 Honjo-machi, Saga 840-8502, Japan; Director, Geopolymer Research Laboratory, 3-3-15 Takakise-nishi, Saga 849-0921, Japan. ORCID: https://orcid.org/0000-0001-6889-5072. Email: [email protected]

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Production of High Compressive Strength Geopolymers Considering Fly Ash or Slag Chemical Composition

Abstract

Introduction

Materials

Preparation of Geopolymer Materials

Chemical Compositions of Geopolymer Materials

Making Geopolymer Samples

Tests and Results

Discussions

Determination of $w_{opt}$ , $η_{opt}$ , and $q_{u \max}$

Correlation between $η_{o p t}$ and Chemical Compositions of Binders

Correlation between $q_{u \max}$ and Chemical Compositions of Binders

Relationship between $q_{u \max}$ and $η_{opt}$

Shrinkage of Geopolymer Samples

Conclusions

Notation

Acknowledgments

References

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Abstract

Introduction

Materials

Preparation of Geopolymer Materials

Chemical Compositions of Geopolymer Materials

Making Geopolymer Samples

Tests and Results

Discussions

Determination of wopt, ηopt, and qumax

Correlation between ηopt and Chemical Compositions of Binders

Correlation between qumax and Chemical Compositions of Binders

Relationship between qumax and ηopt

Shrinkage of Geopolymer Samples

Conclusions

Notation

Acknowledgments

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Determination of $w_{opt}$ , $η_{opt}$ , and $q_{u \max}$

Correlation between $η_{o p t}$ and Chemical Compositions of Binders

Correlation between $q_{u \max}$ and Chemical Compositions of Binders

Relationship between $q_{u \max}$ and $η_{opt}$