DOI: 10.1002/cepa.

843

F U L L PA P E R

Influence of gypsum and limestone, used as mineral additives,

on autoclaved aerated concrete properties

Marek Małecki1 Wiesław Kurdowski2 Paweł Walczak1

1 Department of Research and Development,

Solbet Sp. z o.o., Solec Kujawski, Poland Abstract

2 Glass and Building Materials Division in Gypsum is a very popular mineral additive used in autoclaved aerated concrete (AAC) technol-
Cracow, Kraków, Poland ogy. In many studies, tobermorite can be synthesized from calcium-silicate-hydrate (C-S-H) phase
Correspondence under hydrothermal conditions in the presence of gypsum, and its impact on the tobermorite
Paweł Walczak, Solbet Sp. z o.o., ul. Toruńska 71, content in the AAC blocks has been discussed. It has been found in a previous study that tober-
86-050 Solec Kujawski, Poland.
Email: [email protected]
morite can be synthesized from katoite (Ca3 Al2 [SiO4 ]3-x (OH)4x , where x = 1.5–3.0). Probably, it
is the reason why Al additives accelerated tobermorite formation in the AAC process. Another
very popular mineral additive is limestone. Calcite, in particular limestone, accelerates the reac-
tion between alite with water and forms C-S-H phase, which may have an impact on tobermorite
formation under hydrothermal treatment. The impact of limestone and gypsum as additives on
phase composition and properties of AAC was determined. In the initial study on the laboratory
scale, influence of limestone on the microstructure of AAC was determined. Later, on a techni-
cal scale, properties such as compressive strength, dry density, thermal conductivity coefficient,
drying shrinkage, and phase composition for blocks of AAC containing gypsum additive or calcite
additive were studied.

KEYWORDS
autoclaved aerated concrete, C-S-H, limestone, tobermorite

1 INTRODUCTION Krzheminskij [12,13]. Studies by Baltakys [14] showed that gypsum as

an additive has a good impact on crystallization of tobermorite and pre-
Gypsum is commonly used as a mineral additive in production of auto- vents the formation of xonotlite. Isomorphic substitutions of sulfate
claved aerated concrete (AAC) in sand and fly ash technologies. Inde- ions in hydrated calcium silicates structure resulted in morphological
pendently from used technology, one of the major raw materials is changes in created crystals [15,16]. Observation under a scanning elec-
burned lime, which hydrated in the first stage of production process— tron microscope (SEM) shows differences in the texture of tobermorite
already in the mixer. Additive of sulfate ions, such as gypsum, or compo- with and without sulfate ions. Different results have been observed by
nents of cement have an influence on the hydration of lime [1,2]. In case Schober [17]. In this study, anhydrite was used as a source of sulfate
of the available sand technology, sulfate ions caused a fastest crystal- ions. Anhydrite as an additive does not change the C-S-H phase, but
lization of ettringite and monosulfate [3,4], which have a positive influ- has influence on microporosity. There are many papers available dis-
ence on early compressive strength of a green cake of AAC. cussing about hydration under hydrothermal conditions, but not many
Influence of gypsum on hydration under hydrothermal conditions, publications exist discussing about the influence of tobermorite forma-
phase composition, and microstructure was analyzed in many stud- tion, from the C-S-H phase, on the compressive strength of the building
ies. In the presence of sulfate ions, a faster formation of the C-S- materials. Dyczek [18] studied the influence of the summary content of
H phase and tobermorite can be observed due to decomposition of the C-S-H phase and tobermorite on the compressive strength of the
HE (Ca10 (SiO4 )3 (SO4 )3 (OH)2 ), and katoite (Ca3 Al2 [SiO4 ]3-x (OH)4x ), mortars under hydrothermal conditions. Taylor [19] showed the influ-
where x = 1.5–3.0 [5,6], as described by Sakiyama et al. [7]. Pertlik [8] ence of the compressive strength on concrete paste porosity, and fine-
suggests that one of the final products of hydration is HE with high gyp- ness of cement, fly ash, and quartz after autoclaving. In recent years,
sum content (15–35%). The faster crystallization of the C-S-H phase influence of the CaO/SiO2 ratio on the phase composition, microstruc-
and tobermorite was described by Vektaris [9,10], Grabko [11], or ture, and properties of AAC has been studied [20].


c 2018 Ernst & Sohn Verlag für Architektur und technische Wissenschaften GmbH & Co. KG, Berlin.

ce papers. 2018;2:231–234. wileyonlinelibrary.com/journal/cepa 231

232 MAŁECKI ET AL .

TA B L E 1 Concrete mortars composition

Raw material Sample 1 Sample 2 Sample 3

Cement (g) 13 13 13
Burned lime (g) 13 13 13
Gypsum (g) 2 1 0
Limestone (g) 0 1 2
Quartz (g) 72 72 72

TA B L E 2 Samples composition—technology scale

Raw material AAC 1 AAC 2 AAC 3 AAC 4

Cement (%) 16 16 16 16
Burned lime (%) 5 5 5 5
F I G U R E 1 Phase composition of AAC sample in laboratory stage
Gypsum (%) 0 4 2 0
T, tobermorite; H, hydrogarnet; Kt; Katoite
Limestone (%) 0 0 2 4
Quartz (%) 79 75 75 75

The next very popular mineral additive is a limestone, which con-

sist of calcite, which speeds up reaction of alite with water [21] and
facilitates creation of the C-S-H phase [22]. There is a probability that
additive of calcite will speeds up the conversion of the C-S-H phase into
tobermorite.

2 RESEARCH PROGRAM

In all stages of the study, same raw materials were used as follows:

– ordinary Portland cement CEM I 42,5N,

– burned lime,
– gypsum,
– limestone with fineness <100 𝜇m,
– quartz sand with fineness <200 𝜇m. FIGURE 2 Spherical crystals of anhydrite in Sample 1

2.1 Laboratory stage

age, thermal conductivity coefficient, and phase composition by XRD
On the laboratory scale, three different concrete mortars were com- method were tested.
pared, whose compositions are shown in Table 1.
All samples were prepared with the same water/solid coefficient
and the same amount of the aluminum powder. After casting, samples 3 RESULTS
were conditioned at temperature 25◦ C for 4 h and then autoclaved at
temperature 190◦ C for 8 h. Phase composition by XRD (X-ray diffrac-
3.1 Laboratory stage
tion method) method and observation under SEM were performed for
all samples. Tobermorite with katoite and anhydrite are the main products of
hydration in sample 1 and in this sample limestone with lower peak of
tobermorite can also be observed (Figure 1).
2.2 Technology stage
The microstructure of samples was observed under an SEM, where
On the technical scale, the study was conducted in the one of the AAC spherical crystals of the anhydrite (Figure 2), which stay after decom-
plants. Compositions of all samples are shown in Table 2. position of gypsum, are unstable under hydrothermal conditions. Well-
All samples were prepared with the same water/solid coefficient crystalized fibers of C-S-H phase and tobermorite confirm that they
and the same amount of the aluminum powder. After cutting, sam- are the main product of AAC, as shown in Figure 3.
ples were autoclaved under hydrothermal conditions at temperature High content of scawtite has been observed in Sample 3 with lime-
190◦ C for 8 h. Dry density, compressive strength, drying shrink- stone. Scautite phase creates large clusters of needles (Figure 4), which
MAŁECKI ET AL . 233

TA B L E 3 Test results at the technology scale

Raw material AAC 1 AAC 2 AAC 3 AAC 4

3
Dry density (kg/m ) 490 485 495 500
Compressive strength (N/mm2 ) 2.0 2.9 2.6 2.2
Drying shrinkage (mm/m) 0.34 0.24 0.26 0.34
Thermal conductivity 0.130 0.140 0.135 0.130
coefficient 𝜆 (W/mK)

FIGURE 3 Sample 1 SEM

FIGURE 5 Phase composition comparison—technology scale

The highest amount of tobermorite has been observed in sample

AAC 2 with gypsum. In samples AAC 1 and 4, calcite was observed,
which suggests that in case of sample AAC 4 limestone has not reacted
under hydrothermal conditions, such as calcium hydroxide in sample
AAC 1.

4 CONCLUSIONS

In this study, the impact of limestone and gypsum on the phase compo-
sition, microstructure, and properties of AAC have been studied. Lime-
stone as an additive has an impact on phase composition of AAC by
possible creation of scautite, and it also does not give as good results
as gypsum.
FIGURE 4 Scawtite in Sample 3

ORCID
are the product of reaction between calcite and quartz, as suggested in
Paweł Walczak http://orcid.org/0000-0002-4857-5167
the study of Kurdowski and Pilch [23].

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