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Article history: Plaster and composites made up of gypsum have been widely used in building for different purposes. In
Received 3 February 2016 this work, a new gypsum composite containing diatomite and polypropylene fibers was produced.
Accepted 22 March 2016 Diatomite, fossilized of microscopic plants, was used up to 20% while fiber up to 1%. Samples with
120 120 20 mm and 40 40 160 mm size were produced to do tests. In addition to XRF, XRD,
TGA and SEM investigations of diatomite, physical, mechanical and thermal test were done on produced
Keywords: samples. Also, Analysis of Variance (ANOVA) test were done in order to see the effect of diatomite and
Gypsum
fibers studied on the quadratic model. It was observed that the usage of diatomite increases porosity that
Diatomite
Fibers
results in decreasing unit weight and thermal conductivity coefficient. Fibers increase mechanical
Composite properties.
Plaster Ó 2016 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.conbuildmat.2016.03.125
0950-0618/Ó 2016 Elsevier Ltd. All rights reserved.
O. Gencel et al. / Construction and Building Materials 113 (2016) 732–740 733
and porous structure which is desired for thermal performance, Compounds Diatomite
fire resistance and sound absorption, that makes it attractive for SiO2 75.1
use as a lightweight construction material. Due to its low density, Al2O3 8.37
diatomite can be used as a constituent of concretes and plasters. CaO 2.35
The use of diatomite in gypsum mix should allow a reduction of MgO 0.55
Fe2O3 1.93
the density and thermal conductivity values of the gypsum com- K2O 0.58
posites. Existing studies use different fiber type, while no results Na2O 0.03
have been reported for using both diatomite and polymeric fibers TiO2 0.32
in gypsum composites. Thus, in this study, gypsum composites Loss on ignition 10.5
containing diatomite and polypropylene fibers were produced to
investigate their thermal conductivities, physical and mechanical
properties. 2.4. Preparation and testing of the gypsum composites
Experimental set and mix proportions of the gypsum composite are presented
in Table 4. The gypsum mixtures containing with diatomite and PP fibers were pre-
2. Experimental studies
pared in a mixer. The gypsum and additives were first put in the mixer and mixed
for 5 min in order to achieve a homogeneous dry mixture. Water was then added to
2.1. Gypsum
the dry mixture and mixed for 3 min so as to obtain the plaster slurry. The ratio of
plaster mix/water used was 900 g/585 ml. The water used during these experi-
A commercially available gypsum plaster mix characterized according to TS EN
ments was the room temperature of about 20 °C. Two different shaped molds with
13279-1 [23] was used in this study. The properties of gypsum used were given in
dimensions of 120 120 20 mm and 40 40 160 mm were prepared to pro-
Table 1.
duce test samples. Rectangular (40 40 160 mm) and plate shape
(120 120 20 mm) samples were formed by slurry casting for the mechanical
tests and thermal conductivity determination, respectively. For each test, three ser-
2.2. Diatomite
ies of specimens were produced. In the meantime, the slurry was compacted by a
shaker for 10 s in order to ensure complete filling of the mold. All the specimens
In this study, diatomite for gypsum composite production obtained from Selko
were kept in molds for 24 h at room temperature, and then removed from molds.
A.S. manufacturer in Bartin, Turkey was used. It was characterized for chemical
The specimens were left to dry in ambient conditions for 28 days, further dried in
(X-ray fluorescence analysis), mineralogical (X-ray diffraction analysis), thermal
an oven maintained at 40 °C for 48 h. Dry unit weight values of the samples were
(thermogravimetric analysis) and microstructural (scanning electron microscopy
measured after drying steps. Then porosity and water absorption values, mechani-
analysis) properties.
cal properties like compressive and bending strengths and thermal conductivity
The diatomite particles smaller than sieving intervals of 100-mesh (149 lm)
were determined (Table 5).
were used for mixes. The chemical and physical properties of diatomite are pre-
Compressive and bending strengths, of the gypsum composite samples were
sented in Table 2. Diatomite was added to the mixtures at ratios of 10% and 20%.
determined according to TS EN 13279-2 [24]. The dry unit weight, porosity and
The amount of diatomite listed is the ratio of the diatomite mass to the total dry
water absorption values were determined by Archimedes method (soaking period
mass.
of 24 h in water at room temperature). In order to determine the thermal conduc-
The microstructure of diatomaceous earth is shown in Fig. 1. They have differ-
tivity of the samples a TCi Thermal Conductivity Analyzer has been used. This
ent morphological structures such as cylindrical and others. Their particle sizes are
instrument has been developed by C-Therm Technologies and it is based on the
smaller than 25 lm. The individual particles commonly include submicron sized
Modified Transient Plane Source (MTPS) method, a non-destructive technique
pores. The surface area of diatomite was measured as 13.925 m2/g by a B.E.T. sur-
allowing us to obtain the thermal conductivity and effusivity of the samples tested
face area analyzer. Semi-quantitative chemical analysis of diatomite grains were
[25,26].
determined by the energy-dispersive X-ray spectroscopy (EDS). According to EDS
analysis, the chemical composition of diatomite is 92.7 ± 0.5% SiO2, 6.09 ± 0.4%
Al2O3 and 1.2 ± 0.1% CaO. Also, X-ray fluorescence (XRF) analysis of diatomite was
performed. The analysis result is given in Table 2. The diatomite includes mainly sil-
3. Results and discussion
icon oxide, also the oxides of aluminum, calcium, iron and others. Loss on ignition of
diatomite is about 10.5% by weight. 3.1. Unit weight
Fig. 2 shows X-ray diffraction analysis of the diatomite. The broad hump in the
vicinity of the cristobalite and quartz peaks (from 20° to 40°) is typical for diato-
The unit weights of produced gypsum composites were pre-
mite. This case indicates an amorphous phase (opaline silica) as well as crystalline
silica phases. sented in Fig. 4. As seen from Fig. 4, the unit weight values of the
The TGA curve of diatomite is given in the Fig. 3 where a total weight loss of composites varied between 1007.3 and 881.5 kg/m3 by depending
about 11% for 1100 °C. In the first weight loss, the dehydration of the diatomite on composition. The highest value was observed in reference gyp-
takes place between 20 and 200 °C which corresponds to the loss of free water sum mixture (A1) as 1007.3 kg/m3. The lowest value belongs to the
physically absorbed on the surfaces and in the pores of diatomite particles. The
mass losses in the range of 200–500 °C can be attributed to the removal of chemi-
mixture C3 including 20% diatomite and 1% fiber. As clearly under-
cally absorbed water molecules of amorphous opaline silica (SiO2nH2O). stood from Fig. 4, unit weight decreases in the increment of diato-
mite and fiber concentration in the mixture. The effect of diatomite
is dominant than that of fibers. The effect of fibers is only around
2.3. Polypropylene fibers
1%. The reason behind decreasing unit weight is that diatomite
Polypropylene fibers with 22 lm diameter and 12 mm length were used, their has a lower density due to its porous structure and its concentra-
properties listed in Table 3. The fibers were added into the mixtures in the ratios of tion in the mixture. When diatomite and fibers are used in the ratio
0.5 wt.% and 1 wt.%. The amount of fibers is counted as a ratio to the total dry mass. of 20% and 1%, respectively, unit weight decreases 12.5%. The rela-
tion between unit weight and porosity is presented in Fig. 5.
The ANOVA tests also were done for the unit weight data based
Table 1
The properties of gypsum used.
on the quadratic model. The design referred to quadratic model
with R-squared of 0.9983 and standard deviation of 2.94. The
Workability time (min) 60–90 ANOVA test results for the dry unit weight data are given in Table 6.
Final setting time (min) 150
Compressive strength (MPa) 2.5
The sum of squares is used as a measure of overall variability in the
Flexural strength (MPa) 1 data. Mean square values are obtained by dividing the sum of
Dry density (kg/m3) 650–1000 squares by the degrees of freedom. The model F-value of 357.07
1000 lm (% passing) 100 implies the model is significant. There is only a 0.02% chance that
150 lm (% passing) 60
a Model F-Value this large could occur due to noise. Values of
734 O. Gencel et al. / Construction and Building Materials 113 (2016) 732–740
Table 4
Mixture proportions.
‘‘Prob > F” less than 0.05 indicate model terms are significant. In
this case, A, B, AB and A2 are significant model terms.
Final equation in terms of coded factors for dry unit weight
(UW), Eq. (1):
kg
UW ¼ þ958:7 48:67 A 12:83 B 5:15 A B
m3
Fig. 2. XRD pattern of the diatomite. 8:40 A2 0:8 B2 ð1Þ
3.2. Porosity
Table 5
Experimental results of the gypsum based composite samples.
Mix code Unit weight Porosity (%) Water Ultrasound (m/s) Bending Compressive Thermal
(kg/m3) absorption (wt.%) strength (MPa) strength (MPa) conductivity (W/m K)
A2 999.0 35.9 39.2 579.7 0.8 1.1 0.494
A3 989.0 36.3 39.6 575.9 1.0 1.4 0.495
B1 967.7 43.1 43.8 542.8 0.5 1.4 0.464
B2 958.9 44.6 44.8 540.9 0.6 1.6 0.450
B3 947.9 45.8 45.2 538.4 0.7 1.8 0.455
C1 920.4 47.4 50.4 508.4 0.8 1.6 0.390
C2 901.4 46.9 51.3 509.4 0.9 1.9 0.387
C3 881.5 47.8 52.1 508.1 1.2 2.3 0.384
Fig. 4. Response surfaces for the model given in Eq. (1) for the unit weight.
Table 6
Analysis of Variance (ANOVA) for Response Surface Quadratic Model for the dry unit weights with R2 = 0.9983.
Fig. 6. Response surfaces for the model given in Eq. (2) for the porosity.
Table 7
Analysis of Variance (ANOVA) for Response Surface Quadratic Model for the porosities with R2 = 0.9897.
Fig. 7. Response surfaces for the model given in Eq. (3) for the water absorption.
The compressive strength values of gypsum composites pro- Thermal conductivity values of gypsum composites are pre-
duced vary between 0.9 MPa and 2.3 MPa as presented in Fig. 11. sented in Fig. 12. Thermal conductivity value decreases depending
The highest value was observed in mixture C3 with 2.3 MPa. The on diatomite concentration in the mixture. This means that
lowest value belongs to the mixture A1. Use of diatomite at %10 thermal performance of composites increases up to 63.8%. The
ratio in the mixture increases compressive strength up to %55.6. highest value was obtained as 0.497 W/mK which belongs to A1.
Use of diatomite at %20 ratio in the mixture increases compressive The lowest value was seen in C3 as 0.384 W/mK. The reason behind
strength up to %77.8. This can be attributed to pozzolanic activity it is that density decreases significantly with increasing diatomite
between Ca(OH)2 and diatomite. Also fibers have an effect on com- in the mixture. Also diatomite increases porosity. The increment in
pressive strength of gypsum composites. When fibers are used at % porosity results in decreasing thermal conductivity value. This
0.5 and 1% ratios, compressive strength of gypsum composites relation is shown in Fig. 13. This shows that diatomite can be used
without diatomite increases 22.2% and 55.6%. When looked at to produce plaster and gypsum block element for heat isolation in
combined effect of diatomite at10% ratio and fibers at 0.5% and building constructions. There is no effect of fibers on thermal con-
1% ratios compressive strength increases 77.8% and 100%. Effect ductivity of composites.
Table 8
Analysis of Variance (ANOVA) for Response Surface Quadratic Model for the water absorption with R2 = 0.9974.
Fig. 9. Response surfaces for the model given in Eq. (4) for the ultrasound.
Table 9
Analysis of Variance (ANOVA) for Response Surface Quadratic Model for the ultrasound test with R2 = 0.9987.
Fig. 10. Response surfaces for the model given in Eq. (5) for the bending strength.
Table 10
Analysis of Variance (ANOVA) for Response Surface Quadratic Model for the bending strength with R2 = 0.9133.
Fig. 11. Response surfaces for the model given in Eq. (6) for the compressive strength.
Table 11
Analysis of Variance (ANOVA) for Response Surface Quadratic Model for the compressive strength with R2 = 0.9898.
Fig. 12. Response surfaces for the model given in Eq. (7) for the thermal conductivity.
Table 12
Analysis of Variance (ANOVA) for Response Surface Quadratic Model for the thermal conductivity with R2 = 0.9977.
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