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Thermal, Electrical and Mechanical Properties of Filler-Doped Polymer
Thermal, Electrical and Mechanical Properties of Filler-Doped Polymer
h i g h l i g h t s
a r t i c l e i n f o a b s t r a c t
Article history: The use of filler materials in industrial polymers is becoming increasingly widespread in order to over-
Received 1 February 2019 come the disadvantages of polymers loss of strength. This study proposed a methodology to analyze
Received in revised form 19 July 2019 the effect of filler-doped polymers on the concrete features. The results of the study showed that
Accepted 20 July 2019
Barium Sulfate (BaSO4) doped polypropylene added concrete with 30% polymer/cement ratio has
Available online 30 July 2019
51.03% lower thermal conductivity and 147.99% higher 28-day compressive strength than the reference
concrete. It is determined that Calcium Carbonate doped polyethylene (CaPE) and glass fiber doped
Keywords:
polypropylene (GFPP) gave the highest electrical resistance to the concrete.
Compressive strength
Filler doped polymer concrete
Ó 2019 Elsevier Ltd. All rights reserved.
Multi-response optimization
Thermal conductivity
Electrical resistivity
https://doi.org/10.1016/j.conbuildmat.2019.07.256
0950-0618/Ó 2019 Elsevier Ltd. All rights reserved.
V.A. Küçük et al. / Construction and Building Materials 226 (2019) 188–199 189
Table 2
The properties of filler doped polymers.
4. PERFORMING THE
• Determine test conditions
EXPERIMENT
Fig. 2. a) Compressive strength test apparatus and b) Thermal conductivity test of FIPOCRETE samples.
calcium carbonate doped polymers (A) and content of calcium car- 4. Results and discussion
bonate doped polymer (B) were defined as factors with three levels
and for filler doped polymer (FIDOPO), type of filler doped into the 4.1. Variance analysis
polypropylene (X1) and content of filler doped into the polymer
(X2) were defined as factors with three levels (Table 4). Results of analysis on factor effects [22] and related p-values
A laboratory type mechanical mixer of 5 L capacity was used for given in Table 5 demonstrate that the type of doped polymers
preparing FIPOCRETE. Mixing was completed approximately in are effective on electrical resistance (p-values are 0.001 and
4 min. In order to achieve a better mixture, cement, filled polymers 0.000) CaPE and GFPP type polymers show higher electrical resis-
and two-third of the required water were mixed thoroughly. Then tivity, while CaPP and BaPP type polymers show lower electrical
superplasticizer was added to the mixture with remaining water. resistivity (Fig. 3a and b).
Desirability function and full factorial design methods were used 3 day and 7 day thermal conductivity values show that calcium-
for the implementation of the experiments. doped polymers are effective on thermal conductivity It was deter-
Full factorial design method enables it to investigate one way mined that CaPP type polymer is the most effective polymer on
and two way interaction effects. Experimental runs of full factorial thermal conductivity of concrete (Fig. 4a and b).
design were carried out according to Appendices A-Table A1 All levels (bounds) of types of polymers and content of poly-
(columns 2–3). Mixture details are given in Table A1, columns mers factors have similar effect on the 28 day thermal conductivity
4–7. Results of the experiments are given in Appendices of concrete (Table 5). According to the result of analysis on 28-day
A-Table A2 and A3 for calcium doped polymers and filler doped thermal conductivity values, it was determined that CaPP and
polypropylene, respectively. especially BaPP type the polymers are the most effective types to
V.A. Küçük et al. / Construction and Building Materials 226 (2019) 188–199 191
Table 3
Quality criteria of FIPOCRETE.
Abbr. Definition of the test Test was applied on Target Weightsa Normalized weights
R1 Electrical resistivity (ohm*m) at 28-day Hardened concrete Larger is better 1 0.142857
R2 Thermal conductivity (W/m*K) at 3-day Hardened concrete Larger is better 1 0.142857
R3 Thermal conductivity (W/m*K) at 7-day Hardened concrete Larger is better 1 0.142857
R4 Thermal conductivity (W/m*K) at 28-day Hardened concrete Larger is better 1 0.142857
R5 Compressive strength (MPa) at 28-day Hardened concrete Larger is better 1 0.142857
R6 Water absorption rate (%) Hardened concrete Smaller is better 1 0.142857
R7 Slump flow (cm) Fresh concrete Larger is better 1 0.142857
Total 7 1
a
Identical weight has assigned to all criteria.
Table 4
Factors and their levels for FIPOCRETE.
Table 5
Effects of factors for responses.
Source R1 R2 R3 R4
Term T (Effect) p-value T (Effect) p-value T (Effect) p-value T (Effect) p-value
A 4.33 0.001* 4.15 0.001* 3.34 0.005* 5.34 0.000*
B 0.54 0.596 2.07 0.058 0.62 0.548 3.03 0.009*
A*B 0.79 0.441 0.31 0.764 0.75 0.464 0.52 0.613
X1 5.27 0.000* 0.86 0.402 1.41 0.179 2.41 0.030*
X2 0.60 0.561 0.08 0.938 1.07 0.303 1.81 0.092*
X1*X2 1.45 0.168 1.89 0.079 1.07 0.304 3.39 0.004*
Source R5 R6 R7 N/A
Term T (Effect) p-value T (Effect) p-value T (Effect) p-value N/A N/A
A 0.62 0.547 0.06 0.954 1.12 0.280 N/A N/A
B 0.87 0.401 3.78 0.002* 3.60 0.003* N/A N/A
A*B 2.48 0.026* 1.44 0.172 1.38 0.190 N/A N/A
X1 3.36 0.005* 1.02 0.325 0.74 0.474 N/A N/A
X2 0.37 0.719 8.98 0.000* 2.94 0.011* N/A N/A
X1*X2 0.41 0.690 1.50 0.156 0.54 0.597 N/A N/A
*
Significant at 95% confidence level (p-value < 5/100); positive sign of T-value denotes the synergistic effect and negative sign denotes antagonistic effect.
A B X1 X2
550 325
Mean for R1 (ohm*m)
Mean for R1 (ohm*m)
500 300
450 275
400 250
350 225
300 200
250 175
200 150
CaPE CaPS CaPP 10 20 30 GFPP TaPP BaPP 10 20 30
Type Percentage (%) Type Percentage (%)
Fig. 3. Main effect plots for electrical resistance R1 (ohm*m) a) calcium doped polymer, b) filler doped polypropylene.
decrease the thermal conductivity of concrete (Fig. 5a and b). Highest improvement in compressive strength was achieved
Additionally, it was also determined that type of the polymer dope with BaPP type polymer (Fig. 6a and 6b). Results of the analysis
is effective (p-value 0.005) on the compressive strength of concrete on water absorption percentage and slump value shows that poly-
(Table 5). mer content has higher effect on these criteria than polymer type.
192 V.A. Küçük et al. / Construction and Building Materials 226 (2019) 188–199
A B X1 X2
0.78 0.75
Fig. 4. Main effect plots for thermal conductivity (W/m*K) a) calcium doped polymer, 3-days thermal conductivity, b) filler doped polypropylene 7-days thermal
conductivity.
A B X1 X2
0.70 0.55
Mean for R4 (W/m*K)
0.40
0.60
0.35
0.55 0.30
0.25
CaPE CaPS CaPP 10 20 30 GFPP TaPP BaPP 10 20 30
Type Percentage (%) Type Percentage (%)
Fig. 5. Main effect plots for 28-days thermal conductivity (W/m*K) a) calcium doped polymer, b) filler doped polypropylene.
A B X1 X2
17 29
Mean for R5 (MPa)
28
Mean for R5 (MPa)
16 27
26
15
25
14 24
23
13 22
21
12 20
CaPE CaPS CaPP 10 20 30 GFPP TaPP BaPP 10 20 30
Type Percentage (%) Type Percentage (%)
Fig. 6. Main effect plots for 28-days compressive strength (MPa) a) calcium filled polymer, b) filler doped polypropylene.
Table 6
Mix design for comparison.
Fig. 7. Surface plots for calcium doped polymer in uncoded values, (a) electrical resistance (ohm*m) (b) 28-days thermal conductivity (W/m*K) and (c) 28-days compressive
strength (MPa).
Fig. 8. Surface plots for filler doped polypropylene in uncoded values, (a) electrical resistance (ohm*m) (b) 28-days thermal conductivity (W/m*K) and (c) 28-days
compressive strength (MPa).
Fig. 9. Optimizations plot for a. for calcium doped polymer and b. filler doped polypropylene.
Water absorption percentage and slump value was decreased as the effects of doped polymers on the concrete performance, sepa-
the content of doped polymer in the concrete increased (Table 5). rate concrete composites with both doped and undoped
polypropylene were prepared at same polymer/concrete ratio
4.2. Doped polypropylene vs. polypropylene (%30 by mass). Details of mixture design are given in Table 6.
The results of the experiments and, increase/decrease rates
The performance of doped polypropylene in concrete was com- compared to the undoped polypropylene concrete composite are
pared with undoped (pure) polypropylene. In order to determine summarized in Appendices A-Table A4. Doped polypropylene;
194 V.A. Küçük et al. / Construction and Building Materials 226 (2019) 188–199
shows lower electrical resistance, higher thermal conductivity, with the reference concrete. In addition, compared to reference
lower water absorption as well as significantly higher mechanical concrete, doped polymers admixtures have reduced the percentage
strength compared to undoped polypropylene. of water absorption of concrete composites in contrast to
When doped polypropylene is compared to polypropylene, it polypropylene admixture. The lowest the water absorption rate
can be seen that GFPP caused the least electrical resistance is 18.33% is achieved with TaPP admixture (Appendices A-
loss (53.22%) while BaPP caused the least thermal resistance Table A4).
loss (17.96%). With TaPP, much higher compressive strength
(209.42%) and lower water absorption rate (20.60%) were obtained
4.3. Optimum design
compared to polypropylene (Appendices A-Table A4).
When the properties of the doped polypropylene concrete com-
In full factorial design approach, three-dimensional plots are
posite and the properties of the reference concrete are compared, it
used to predict the connection of responses and factors and to
was observed that the doped polymers resulted in lower electrical
determine the ‘‘decision point” required for desirability function.
resistance whereas the undoped polypropylene concrete compos-
The ‘‘decision point” of the plot has saddle shape for all responses
ite caused 59.7% higher electrical resistivity. When the 28 days
[22]. The response surface graphs were plotted for two factors
thermal conductivity value is analyzed, it is determined that the
while the third factor was held constant at the middle level (Figs. 7
thermal conductivity of the concrete with undoped polypropylene
and 8).
was 58.48% lower than the reference concrete and thermal conduc-
The desirability function makes it possible to integrate all
tivity of the concrete with BaPP 51.03% lower than the reference
responses under a single function and to obtain ‘‘optimum results”
concrete. However in terms of 28 day compressive strength 30%
with maximizing this function. The responses with different scales
polypropylene admixture caused 12.56% loss in comparison with
can be examined together at the same time and the many
the reference concrete, whereas 30% TaPP admixture has a
responses can be easily transformed into a single function to per-
170.55% improvement in comparison with the reference concrete
form multi-response optimization. Another advantage of the
and the BaPP admixture has a 148% improvement in comparison
method is that it can be easily applied with Minitab software. In
V.A. Küçük et al. / Construction and Building Materials 226 (2019) 188–199 195
order to make it possible to do a multiple-response optimization absorption rate were achieved. On the other hand, 56.09% decrease
using full factorial design, in this study, full factorial design is in electrical resistance was observed.
combined with desirability function approach (Appendices B)
[36–39]. 4.4. Morphological analysis
Individual desirability values, the overall desirability D and pre-
dicted value were also calculated using MINITABÒ version 17 SEM images of the interfaces of polymer and cement paste were
(Appendices B-Table B1). The factors obtained at the saddle points taken for all doped polymer types (Figs. 10 and 11, Blue Square).
of R1, R2, R3, R4, R5, R6 and R7 (each responses have equal weight) It was seen that the doped polymers form a compact structure
were calculated as 108.48 kg CaPE and 101.4 kg GFPP as given in with the cement paste and the filler polymer is attached to the
optimization plot a and b (Fig. 9) [22,36–39]. concrete.
After the determination of optimum levels, validation experi- Leaf-like C-S-H (Calcium-Silicate-Hydrate) gels are seen in all
ments were carried out. Validation experiments were statistically doped polymer concretes at 5.0KX (5000X) magnifications. The
compared with the results of predicted optimum levels using presence of leaf-like C-S-H gels in all SEM images is an indication
paired t-test (Appendices C-Table C1). The accuracy of the results that hydration process of the cement was successful and that con-
verifies the validity of the models [22]. crete will gradually gain strength in the future. Another interesting
For 108.48 kg CaPE usage in concrete composite, 6.19% point is that there are no cracks at the polymer structure and there
improvement in electrical resistance, 17.9% improvement in is no separation from cement paste, structural cracks within the
thermal conductivity and 44.49% improvement in 28-day compres- polymer and separation from cement paste can easily be seen in
sive strength were achieved compared to control samples. On the the images of undoped polymer added concrete (Figs. 10 and 11).
other hand, 2.96% decrease in water absorption rate was observed. There results can be interpreted as the reason for compressive
For 101.4 kg GFPP usage in concrete composite, 35.99% improve- strength improvement in doped polymer added concrete compos-
ment in 28-day thermal conductivity, 83.83% improvement in ites. It should be also noted that no voids were observed in the SEM
28-day compressive strength and 17.84% improvement in water images of GFPP and BaPP concrete composites [11,15,40].
Table A1
Details of the mixtures and experimental design.
Table A2
Experimental results for calcium doped polymer concrete.
Table A2 (continued)
Table A3
Experimental results for filler doped polypropylene concrete.
Table A4
Comparison study with doped polymer.
Exp. No Exp. Code. R1 (ohm*m) R2 (W/m*K) R3 (W/m*K) R4 (W/m*K) R5 (MPa) R6 (%) R7 (cm)
0 REF 488.0 0.613 0.631 0.778 9.71 22.70 18
1 PP30 779.2 0.307 0.329 0.323 8.49 23.35 12
C9 CaPP30 268.5 0.554 0.518 0.495 17.85 22.33 10
P3 GFPP30 364.5 0.556 0.607 0.542 16.95 19.65 10
P6 TaPP30 193.5 0.565 0.583 0.541 26.27 18.54 10
P9 BaPP30 160.5 0.421 0.493 0.381 24.08 19.41 10
According to PP30 Increase or decrease rate1 65.54a 80.46b 57.45 53.25 110.25 4.37 16.7
Increase or decrease rate2 53.22 81.11 84.50 67.80 99.65 15.85 16.7
Increase or decrease rate3 75.17 84.04 77.20 67.49 209.42 20.60 16.7
Increase or decrease rate4 79.40 37.13 49.85 17.96 183.63 16.87 16.7
According to REF Increase or decrease rate5 59.67 49.92 47.86 58.48 12.56 2.86 –33.3
Increase or decrease rate6 44.98 9.62 17.91 36.38 83.83 1.63 44.4
Increase or decrease rate7 25.31 9.30 3.80 30.33 74.56 13.44 44.4
Increase or decrease rate8 60.35 7.83 7.61 30.46 170.55 18.33 44.4
Increase or decrease rate9 67.11 31.32 21.87 51.03 147.99 14.5 44.4
1
For CaPP30,
2
for GFPP30,
3
for TaPP30
4
for BaPP30 according to PP30
5
For PP30,
6
For CaPP30,
7
For GFPP30,
8
For TaPP30 and
9
For BaPP30according to REF
a
268:5779:2
100 ¼ 65:54,
b
0:5540:307
779:2
0:554 100 ¼ 80:46.
198 V.A. Küçük et al. / Construction and Building Materials 226 (2019) 188–199
Table B1
The optimum responses.
Response Description Levels Stationary point Weight Composite desirability Predicted value Optimal D
Lower Target Upper
R1 Electrical resistivity 214 600 746 Saddle 1a 1b 0.15778a 534.91a 0.6054a
(ohm*m) 143 200 370 0.97490b 198.57b 0.7778b
28-days
R2 Thermal conductivity 0.50 0.7 0.83 Saddle 1a 1b 0.82196a 0.7237a
(W/m*K) 0.36 0.5 0.63 0.99583b 0.5005b
3-days
R3 Thermal conductivity 0.45 0.5 0.88 Saddle 1a 1b 0.94232a 0.7103a
(W/m*K) 0.38 0.5 0.67 0.83533b 0.5285b
10-days
R4 Thermal conductivity 0.49 0.5 0.77 Saddle 1a 1b 0.72477a 0.6460a
(W/m*K) 0.36 0.4 0.59 0.59284b 0.4774b
28-days
R5 Compressive strength 8.67 15 20.54 Saddle 1a 1b 0.61282a 12.5492a
(MPa) 16.78 30 36.42 0.74282b 26.6001b
28 days
R6 Water absorption 18.33 20 25.14 Saddle 1a 1b 1.0000a 20.0a
(%) 18.53 20 23.94 0.98463b 20.0606b
R5 Slump flow 8 13 14 Saddle 1a 1b 0.54885a 10.7442a
(cm) 8 13 16 0.48994b 10.4497b
a
Setting the same weight for calcium filled polymer.
b
Setting the same weight for material filled polypropylene.
B: Full factorial design based desirability function approach After the desirability functions are obtained for each of the
responses, their geometric mean is calculated and a single collec-
The desirability function can be described as an index for mul- tive desirability function (D) can be achieved for all of them.
tiple responses ranging from 0 to 1. Where, 1 indicates that opti-
mum values have been determined. Calculation of desirability D ¼ ðd1 d2 d3 dn Þ
1=n
ð2Þ
function is made for each Yi belonging to di and then, the geometric
mean of these particular functions is calculated. Thus a single col-
d1, d2, d3, dn are desirability values of responses and n denotes the
lective desirability function (D) is obtained. Ti states, Li and Ui state
number of total responses. Desirability function (with ‘‘nominal the
target value, limit inferior and superior respectively. S and t are the
best” approach) could be defined for the responses according to
weights demonstrating the importance of responses on target
response surface plots. Bounds determined (lower, upper and desir-
value and on the total desirability role.
able) for the responses are given in Table B1.
8
> 0 ^i ðxÞ < Li
y
>
<h is
^i ðxÞLi
^i Þ ¼
d i ðy y
^i ðxÞ < T i
Li 6 y ð1Þ C: Validation of the optimum levels
>
>
T i Li
:
1 ^ i ð xÞ > T i
y
Table C1
Table C1
T-test results for the verification of the results.
No Response Predicted values Result of validation experiment Difference (d) Standard deviation t-test Statisticsà T6;0.025 (tn-1,a/2)
Mean,d
1 R1 534.91a 518.2a 16.71a 2.3326a 6.3929a *
0.97a 2.447a
198.57b 214.3b 15.73b 2.7151b 5.7705b -1.24b
*
2.447a
2 R2 0.7237a 0.704a 0.0197a
0.5005b 0.554b 0.0535b
3 R3 0.7103a 0.729a 0.0187a
0.5285b 0.511b 0.0175b
4 R4 0.6460a 0.638a 0.008a
0.4774b 0.498b 0.0206b
5 R5 12.5492a 14.03a 1.48a
26.6001b 28.15b 1.5499b
6 R6 20.0a 18.65a 1.55a
20.0606b 21.18b 1.1194b
7 R7 10.7442a 11a 0.26a
10.4497b 11b 0.5503b
Total n=7
a
: Setting the same weight for all responses (CAFIPO).
b
: Setting the same weight for all responses (FIDOPO) (d) = Predicted values – Verification experiment.
*
Null p
hypothesis
ffiffi H0 = There is no significant difference between the two means. Since 0.97 < 2.447 and 1.24 > 2.447, null hypothesis would not reject.
à
t ¼ dSd n.
V.A. Küçük et al. / Construction and Building Materials 226 (2019) 188–199 199
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properties of polypropylene polymers, Korean J. Chem. Eng. 32 (2015)
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