Graduate Seminar for the Degree of Master of Engineering

2018
February 9, St. John’s

THERMAL ENERGY STORAGE WITH PARAFFIN WAX AND

STABILITY STUDY OF THE PHASE CHANGE MATERIAL WITH
NANOPARTICLES

by Vahit SAYDAM

Supervisor: Dr. Xili DUAN

Department of Mechanical Engineering

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Presentation Outline
1. Objectives of the research
2. Helical Coil-LHTESS (Latent Heat Thermal Energy
Storage System) with Paraffin Wax
i. Charging and discharging tests
3. Nano-enhanced Phase Change Material (NEPCM)
i. Materials and sample preparation
ii. Thermal conductivity and DSC measurement
iii. Stability Study
4. Conclusions
5. Recommendations for Future Work
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1. Objectives
• Observe the melting and solidification characteristics of paraffin
wax in a helical coil heat exchanger energy storage under different
operational conditions.

• Determine the effects of HTF flow rate, flow direction and, inlet
temperature on charging and discharging tests.

• Examine the feasibility of using NEPCM as a heat transfer

enhancement in LHTESS.

• Investigate the preparation and characterization of paraffin wax

with various nanoparticles.

• Study the effect of dispersion methods on the stability of NEPCM.

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2. LHTESS with Paraffin Wax

• Experimental Setup
• Charging and discharging tests
– The effect of HTF flow rate
– The effect of HTF inlet temperature on charging
– The effect of HTF flow direction
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Experimental Setup

(a) (b)

Figure 1: (a) Schematic of the experimental setup; (b) Positions of thermocouples; T1: Side
bottom, T2: Center bottom, T3: Center middle, T4: Center Top, T5: HTF Inlet, T6: HTF Outlet
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Charging and discharging tests

Table 1: Outline of the experiments under different operational conditions
Experiment Experiment HTF Flow HTF Inlet Flow
number type rate, LPM temperature, °C direction
Test 1 Charging 4 75 Upward
Test 2 Charging 2 75 Upward
Test 3 Charging 1 75 Upward
Test 4 Charging 0.5 75 Upward
Test 5 Charging 4 70 Upward
Test 6 Charging 4 75 Downward
Test 7 Discharging 2 20 Upward
Test 8 Discharging 1.5 20 Upward
Test 9 Discharging 1 20 Upward
Test 10 Discharging 0.5 20 Upward
Test 11 Discharging 1.5 20 Downward
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Charging
80
70
60
Temperature, °C

50 Inlet

Outlet
40
Center Top
30 A B C
Center Middle
20
Center Bottom
10
Side Bottom
0
0 25 50 75 100 125 150 175 200 225
Time, min

D E F
Figure 2: Charging with a flow rate of 4 LPM Figure 3: Pictures of charging with a
at 75°C inlet HTF temperature flow rate of 4 LPM at 75°C (A:30 min,
B:60 min, C:90 min, D:120 min, E:145
min, F: 170 min)
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Discharging
80
Inlet
70
Outlet
60 Center Top
Temperature, °C

50 Center Middle

40 Center Bottom

Side Bottom
30
20 A B C
10
0
0 100 200 300 400
Time, min
Figure 5: Pictures of discharging
Figure 4: Discharging with a flow rate of 1 LPM at with a flow rate of 1 LPM at 75°C (A:0
20°C inlet HTF temperature min, B:30 min, C:150 min)
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The effect of HTF inlet temperature on charging

80

70

60
Temperature, °C

50

40

30
75°C
20
70°C
10

0
0 25 50 75 100 125 150 175 200 225 250 275
Time, min

Figure 6: Temperature profile of center top thermocouple at different inlet

temperatures with 4 LPM during charging
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The effect of HTF flow rate on charging

80
70
60
Temperature, °C

50
40 4 LPM

30 2 LPM

20 1 LPM

10 0.5 LPM

0
0 50 100 150 200 250
Time, min

Figure 7: Temperature profile of center bottom thermocouple at different flow rates

during charging at 75°C
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The effect of HTF flow rate on discharging

80
2 LPM
70

60 1.5 LPM
Temperature, °C

50 1 LPM

40 0.5 LPM
30

20

10

0
0 50 100 150 200 250 300 350
Time, min

Figure 8: Temperature profile of center top thermocouple at different flow rates

during discharging at 20°C
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The effect of HTF flow direction on charging

80

70

60
Temperature, °C

50

40

30
Upward flow, 4 LPM
20

10 Downward flow, 4 LPM

0
0 20 40 60 80 100 120 140 160 180 200
Time, min

Figure 9: Temperature profile of center bottom thermocouple at different flow

directions with 4 LPM during charging at 75°C
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The effect of HTF flow direction on discharging

70
Upward flow, 1.5 LPM
60
Downward flow, 1.5 LPM
50
Temperature, °C

40

30

20

10

0
0 50 100 150 200 250 300 350
Time, min

Figure 10: Temperature profile of center bottom thermocouple at different inlet

positions with 1.5 LPM during discharging at 20°C
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Charging and Discharging test times

6
Charging at 75°C,
5 upward flow
Charging at 70°C,
4 upward flow
Time, h

Charging at 75°C,
3
downward flow
Discharging at 20°C,
2
upward flow

1 Discharging at 20°C,
downward flow
0
0 1 2 3 4 5 6 7
Flow rate, LPM

Figure 11: Comparison of charging and discharging times for different operational
conditions
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3. Nano-enhanced Phase Change Materials (NEPCM)

• Low thermal conductivity of paraffin wax as a storage

material causes poor heat transfer performance.
• The recovery of the stored energy during discharging is
adversely affected due to conduction dominated heat
transfer within paraffin wax.
• Long charging/discharging times require heat transfer
enhancement methods.
• Dispersing highly conductive nanoparticles into
paraffin wax could provide the required heat transfer
enhancement.
• Therefore, NEPCM are proposed to address this issue.
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Materials

A B C D E F

Figure 11: A: Paraffin wax, B: MWCNTs (6-9 nm in diameter and 5µm in length), C: Aluminum
oxide particles(<50nm particle size), D: Graphene nanoplatelets(lateral dimensions of about 2-3
𝜇). E: Sodium oleate, F: Octadecylamine.
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Sample preparation

Figure 12: Sample preparation using mechanical dispersion method

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Thermal Conductivity Measurements

• Thermal conductivity measurements were made using KD-2 Thermal

Conductivity Analyzer probe at different temperatures by varying the amount
of nanoparticles both in liquid and solid phase in an environmental chamber.

Figure 13: KD2 Pro Figure 14: 3-D printed Figure 15: Environmental Chamber (Tenney
Thermal Conductivity mold for measurements Junior Test Chambers, Model T30RC)
Analyzer(Decagon in solid phase
Devices)
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Thermal Conductivity Measurements

Figure 16: Thermal conductivity change in liquid phase (60°C) over time after sample
preparation
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Thermal Conductivity Measurements

Figure 17: Thermal conductivity change with temperature

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Differential Scanning Calorimetry Measurements
• DSC measurements were conducted using Mettler-Toledo DSC1 device
between 20-80°C at 5 °C/min heating/cooling rate.

Figure 19: Mettler-Toledo DSC1

Figure 18: DSC heating and cooling curves of paraffin wax

with MWCNT, graphene nanoplatelets and Aluminum oxide
nanoparticles at different concentrations.
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Differential Scanning Calorimetry Measurements

Table 2: Phase change temperature and latent heat of fusion of paraffin wax with
various nanoparticles at different mass fractions.

Samples Tm,peak(°C) Ts,peak(°C) ∆T(°C) ∆Hm(J/g) ∆Hs(J/g)

Paraffin wax 54.86 53.02 1.84 124.61 126.85
0.5 wt. % MWCNT-wax 54.09 52.95 1.14 127.53 124.72
1 wt. % MWCNT-wax 52.72 53.1 -0.38 130 127.19
2 wt. % MWCNT-wax 54.77 52.15 2.62 120.34 120.81

0.5 wt. % Graphene-wax 56.18 52.17 4.01 114.74 112.25

1 wt. % Graphene-wax 56.18 52.17 4.01 133.85 134.19
2 wt. % Graphene-wax 55.88 52.44 3.44 115.31 114.57

0.5 wt. % Aluminum oxide-wax 56.19 53.76 2.43 138.17 136.17

1 wt. % Aluminum oxide-wax 56.19 51.94 4.25 94.29 93.62
2 wt. % Aluminum oxide-wax 55.33 52.4 2.93 117.26 116.33
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Stability study-Effect of Sonication time on Stability

Figure 20: Stability observation of Figure 21: Settling of MWCNTs in

MWCNT-paraffin samples in liquid phase over paraffin wax in solid phase
first (1), second (2) and third (3)
melting/solidification cycles (Sample A: 0.1
wt.%,100 min sonication; B: 0.1 wt.%,40 min
sonication; C: 0.075 wt.%,70 min sonication; D:
0.05 wt.%, 100 min sonication; E: 0.05 wt.%,
40 min sonication)
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Stability study-Effect of using surfactants on Stability
• Effect of using Sodium oleate on the stability of nanoparticles over
thermal cycles

Figure 22: Stability observation of various nanoparticles in paraffin wax with sodium oleate
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Stability study-Effect of using surfactants on Stability
• Effect of using Octadecylamine on the stability of nanoparticles
over thermal cycles

Figure 23: Stability observation of various nanoparticles in paraffin wax with octadecylamine
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Stability study-Effect of boundary conditions on Stability
• Effect of bottom heating on the stability of nanoparticles over
thermal cycles #C melting for
2h
solidifying solidifying solidifying solidifying
for 30 min for 60 min for 90 min for 120 min
0

Figure 24:Solidification of 0.1 wt.% MWCNT-wax sample after melting on a hot plate at 150°C
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4. Conclusions
• HTF inlet temperature has the greatest effect on the charging time.
• Switching the flow direction from upward to downward did not have a
significant influence on charging due to uniform temperature along the helical
coil at high flow rates.
• Discharging tests were longer than the charging tests due to poor conduction
heat transfer performance of paraffin wax.
• Mechanical(stirring and sonication) dispersion and surfactant usage did not
help attain stable homogenously dispersed NEPCM samples over
melting/solidification cycles.
• The highest thermal conductivity enhancement was obtained for 2 wt. %
MWCNT-wax sample by 13% at 35°C. The insignificant overall improvement of
thermal conductivity is due to particle deposition and instability associated
with bad dispersion quality.
• DSC study of NEPCM samples showed anomalous latent heat capacity results
without any trend. However, the presence of nanoparticles did have a negative
effect on the supercooling issue.
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5. Recommendations for future work

• For the LHTESS study, alternative techniques of heat transfer enhancement need to be
explored particularly for discharging process where conduction is the main heat transfer
mechanism. Traditional enhancement methods with fins could be revisited.
• Using NEPCM in the LHTESS could be a remedy to existing poor heat transfer
performance of PCM. However, this method seems to be not feasible due to stability
related issues.
• Therefore, multidisciplinary approach is required to achieve good understanding of
physical/chemical properties of PCM and nanoparticles so that long-term stable NEPCM
colloids could be obtained.
• Special porous media with microscale pores may enable overall uniform homogeneous
long-term dispersion of nanoparticles into PCM. It can solve the stability issue of
NEPCM. This technique is currently being investigated in our lab.
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References

• Khodadadi, J. M., Fan, L., & Babaei, H. (2013). Thermal conductivity enhancement of
nanostructure-based colloidal suspensions utilized as phase change materials for thermal
energy storage: A review. Renewable and Sustainable Energy Reviews, 24, 418-444.
• Das, S. K., Choi, S. U., Yu, W., & Pradeep, T. (2007). Nanofluids: science and technology. John
Wiley & Sons.
• Tang, Q., Sun, J., Yu, S., & Wang, G. (2014). Improving thermal conductivity and decreasing
supercooling of paraffin phase change materials by n-octadecylamine-functionalized multi-
walled carbon nanotubes. RSC Advances, 4(69), 36584-36590.
• Sidik, N. A. C., Mohammed, H. A., Alawi, O. A., & Samion, S. (2014). A review on preparation
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• Michaelides, E. E. S. (2014). Nanofluidics: thermodynamic and transport properties. Springer.
• Korti, A. I. N., & Tlemsani, F. Z. (2016). Experimental investigation of latent heat storage in a
coil in PCM storage unit. Journal of Energy Storage, 5, 177-186.
• Kabbara, M., Groulx, D., & Joseph, A. (2014). Experimental study of a latent heat storage unit
with a helical coil heat exchanger. In CSME International Congress 2014, Toronto, Canada.
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Acknowledgements
This research study was funded by NL Innovation Council and
National Research Council of Canada.
Thank you!