4.2. Baseline Testing
In the earlier experimental study, Strandberg and Das [
7] conducted baseline testing to validate the instrumentation and test methodology. That original baseline testing already demonstrated that the test bed generates performance data that are aligned with expectations. Nonetheless, additional testing was performed on the improved test bed to demonstrate that the heat transfer performance measured by the instrumentation agreed with what was expected as determined by the manufacturer’s data and computations based on methods accepted in the literature. The additional testing was to validate that the relocation and minor revisions to the piping did not adversely impact the quality of data generated by the test rig.
Baseline apparatus testing was conducted using water on the “wet” side of the test loop. The test runs were designed to verify that the measured thermal output of the liquid-to-air heating coil agrees with the manufacturer’s product data. The hot water was circulated through the tubes of the heating coil while heating air was drawn through the fins. The test bed instrumentations measured volumetric flow rates and average temperatures in the air and water streams, and the heat transfer rate between the water and air streams was computed from there.
Another objective of the baseline testing was to characterize the energy balance between the air and water streams over the operating envelope of the test. The difference between the rates of heat transfer measured in the two streams was an essential measure of experimental error in the testing apparatus. Quantifying and minimizing the energy imbalance is crucial as it indicates that the energy loss rate to the environment has been controlled and provides the primary check on the performance of the air Venturi meter. By validating the performance of the air Venturi meter, the analysis of nanofluid heat transfer performance will become more straightforward since the thermophysical properties of air are well understood over the range of test conditions, and air properties are also constant over time (at constant temperature and pressure). In contrast to air, the thermophysical properties of nanofluids may change over time due to degradation caused by suspension instability, particle agglomeration, and subsequent settling.
Vajjha and Das’s earlier work [
22] involved property measurements. During those experiments, we used the nanofluids immediately after receiving them from Alfa Aesar [
23]. They were fresh, uniformly dispersed. The sample sizes for viscosity, thermal conductivity, specific heat, and density were small. There was no circulation of nanofluids as these were static tests on small sample volumes confined to a contained space. The experiments were of short duration. So, we measured the optimum property values under ideal conditions.
However, in the present experiments, the nanofluids circulated in a coil for very long durations to obtain data over a range of Reynolds, Prandtl, and Nusselt numbers varying flow rate, temperature, pressure to measure, convective heat transfer, heat transfer rate, pressure loss, and pumping power. Maintaining nanofluid purity was a more significant challenge because we started with an older nanofluid that had lost its uniform dispersion ability. This was unknown to us initially, but the unexpectedly poor performance result taught us a lesson.
The first baseline test was performed in which the volumetric flow rate of the water was varied, while the inlet liquid and air temperatures, as well as the air volumetric flow rate, were all held constant at practical values of 340 K, 289 K, and 0.23 m
3/s, respectively. The result of this testing is illustrated in
Figure 5, with the calculated heat transfer rate for the air and liquid streams. In this test, 708 individual measurements were recorded for both fluid streams. Each data point is the average of several measurements. The average difference between the calculated air- and liquid-side heat transfer rates is 10.0%. The first experiment near Re = 2000 is an outlier in the heat rate difference. Disregarding this first point, the average difference is reduced to about 8%. For additional validation of the empirical measurements, the coil was modeled using identical entering conditions and configuration using the approach described by Strandberg and Das [
7]. The heat transfer rate of the modeled coil over the same range of liquid flows was within 3% of the empirically obtained air rate of heat transfer over the tested range. The average of the liquid and air rates of heat transfer were used for performance comparisons. The test bed was allowed to reach a steady state for each run before data collection.
In the second baseline test, the inlet water temperature was varied, and the volumetric flow rate of the water and air was kept constant. The volumetric flow rate of liquid was held constant at 0.063 L/s while the airflow was constant at 0.222 m
3/s. The result of this test is illustrated in
Figure 6. The difference between the air-side and liquid-side calculated heat transfer rate ranges from 0.23% to 9.4%, with a mean of 3.4%. Here, the fourth data point near 342 K is an outlier. Disregarding this outlier, the average difference between energy balances comes to about 3%, an acceptable value for validating the test bed. For this test, the total number of data points is 902 (with between 64 and 192 observations at each temperature).
The following baseline test was to measure the viscous losses through the hydronic coil over a range of flows. These data are illustrated in
Figure 7. The pressure loss measured through the coil apparatus showed remarkable agreement with the coil manufacturer’s published data [
19] over the practical flow range. This validates the accuracy of the experimental setup for measuring the pressure loss for subsequent runs with nanofluids of different concentrations.
Using the data collected in baseline testing, the “inside” heat transfer coefficient (
hi) was computed as an additional check to verify that measured values aligned with those predicted by well-established correlations in the literature for single-phase liquids. In
Figure 8, the graph depicts the experimentally determined “inside” heat transfer coefficient compared to values computed using the Petukhov correlation [
29] as a function of the Reynolds number. This test was performed with constant air-side velocity and a temperature and pressure range of relatively constant thermophysical properties for air. Therefore, it is a reasonable assumption that the outside heat transfer coefficient over the fins and copper tube will remain relatively constant over the full range of inside liquid volumetric flows. Airflow was constant at 0.230 m
3/s (487 CFM); air and liquid inlet temperatures were also held constant. Liquid flows were varied through the coil from 0.019 to 0.10 L/s (0.3 to 1.5 GPM).
Heat transfer rates for liquid and air were computed using well-established heat exchanger design equations from McQuistion et al. [
25], Bejan [
28], and Shah and Sekulic [
30] using measured volumetric flow rates and temperatures.
The principal equation is
where
is the overall heat transfer coefficient,
is the outside surface area of heat transfer coil,
is the log mean temperature difference,
is the fin efficiency, and subscripts
and
represent inside and outside, respectively.
The
LMTD was calculated from measured inlet and outlet temperatures of fluid streams. The product
UA was also calculated based on
from energy balance. The inside and outside heat transfer coefficients were determined by finding the values of the inside coefficient using the Petukhov correlation and then calculating the outside heat transfer coefficient by rearranging Equation (7). Based on the physical conditions of the test, in which the airflow velocity remains constant, it is acceptable that the property values of air over the range of test runs would remain nearly identical. Using the Petukhov correlation for
hi, rearranging Equation (7), and averaging numerous measurements, the mean value found for
ηhoAo was 193 W/K. At the lowest flows observed, the liquid Reynolds numbers drop (<2300) into the range usually considered “transitional” with respect to the presence of turbulence in the liquid stream. However, the Petukhov correlation was designed for fully turbulent flows (Re ≥ 10,000) and fits the experimentally obtained values in
Figure 8 with R
2 = 0.89. The Petukhov correlation predicts
hi values lower than the empirically determined values from Nusselt numbers using the Gnielinski equation from Bejan [
28] over the tested range. The average deviation between
hi from Petukhov and experimental values via Gnielinski over the tested range is 12.2%. This is acceptable considering that well-known Nusselt number correlations can present uncertainty as high as 25%. Gnielinski’s equation works well in a transition regime, so the agreement in
Figure 8 below, Re = 3500, between the experiment and theory is encouraging.
An important point: the tubing bends create secondary flows even at the laminar regime, promoting mixing and enhancing heat transfer at the Reynolds number in the transition regime, making the entire flow turbulent. At a low laminar Reynolds number, this phenomenon causes the experimental data to match the Petukhov and Gnielinski correlation in
Figure 8, which is applicable to turbulent flows.
The value for
ηhoAo = 193 W/K by averaging process from numerous test runs was only 3.9% lower than what is found using the procedure given in McQuiston et al. [
25], showing good agreement between measured data and previously established correlations. Since the outer thermal resistance will remain essentially unaffected by the properties of the liquid flowing inside the tube, this value is used to evaluate the heat transfer performance of the nanofluids in the performance tests that followed.
4.3. Nanofluid Performance Testing
Nanofluid samples were prepared for multiple test runs with different concentrations of nanoparticles. The authors formulated 60% EG/Al2O3 nanofluids of particle volumetric concentrations of 1%, 2%, and 3% and the base fluid (60% EG). These dispersions were separately fed into the testbed and subjected to a series of performance tests. These tests are designed to characterize the differences in heat transfer performance between the Al2O3/60% EG nanofluid and 60% EG measured during testing. For this series of tests, the liquid and air inlet temperatures were held constant and liquid volumetric flow rates were varied.
In order to minimize the contamination of the fluids, between each series of tests, the loop was drained, refilled with water, and cleaned out until the rinse water came out clear. The tubing was partially disassembled and allowed to drain. Finally, all sections were blown out with high-pressure compressed air to clean out residual fluids. Upon completion, the system was refilled with fresh test fluid.
In
Figure 9, the inside heat transfer coefficients for the base fluid (60% EG) are compared to those for the Al
2O
3/60% EG nanofluids for liquid volumetric flows ranging from approximately 0.025 to 0.2 L/s (0.4 to 3.2 GPM). The inside heat transfer coefficient was found by first computing the measured rate of heat transfer and
LMTD based on the measured data and then determining the value for UA.
As explained in
Section 4.2, the outside thermal resistance (
ηhoAo) is accepted to have a value of 193 W/K, as determined in the baseline test. The inside heat transfer coefficient was then calculated considering the inside surface area of the heat transfer section.
Previous experimental work by Strandberg and Das [
7] comparing the heat transfer performance of 60% EG to 1% 60% EG/Al
2O
3 did not show a significant improvement in the heat transfer performance of the nanofluid relative to the base fluid. This was attributed to the relatively low temperature of the liquid tested, which was limited by the heat source connected to the test equipment. The data in
Figure 9 depicting the empirically determined inside heat transfer coefficients for the tested dispersions show that as the nanofluid concentration increases, the inside heat transfer coefficients decrease under equal volumetric flow rate conditions.
In the current experiment, the heat transfer coefficient decreases by 5.7%, 23.0%, and 44.3% for 1%, 2%, and 3% Al
2O
3/60% EG nanofluids, respectively, compared to the 60% EG base fluid, at a constant flow of 0.15 L/s (2.4 GPM). Due to nanofluids’ relatively higher viscosity, the Reynolds number at a given volumetric flow is generally lower than for the base fluid. According to well-established equations, the Nusselt number and the convective heat transfer coefficient are proportional to the Reynolds number for internal flows. Therefore, it is to be expected that the heat transfer coefficients for nanofluids are lower than for the base fluid when compared on a constant volumetric flow basis. Note in the legend of
Figure 9 that two data sets for 60% EG were taken on different days.
Early in the test cycle, after the nanofluids’ relatively low thermal performance was observed, the authors attempted to verify that the thermophysical properties of the dispersion were as expected based on the previously cited correlations. To this end, representative dispersions samples were tested in a Brookfield viscometer at room temperature. These tests produced conflicting results in which the measured viscosities of the nanofluids did not correlate well with predicted values. Generally, the nanofluids’ measured viscosities were higher than the correlation of Vajjha and Das [
21] predicted. This makes comparisons between fluids based on the Reynolds number challenging to hold in high confidence since the value is computed using a value for viscosity that cannot easily be directly determined at the time of the experiment. As a result, comparisons are reported based on volumetric flow instead of on Reynolds number.
Figure 10 presents graphically the Nusselt numbers for the base fluid and the nanofluids over the range of flows tested. As with the heat transfer coefficient and heat rate data, these data similarly contradict the results predicted by the earlier analytical model. At a volumetric flow rate of 0.125 L/s, the predicted value for the Nusselt number of the 60% EG was 61.3. Based on the testing, the 60% EG circulating at 0.125 L/s exhibited a Nusselt number of 70. The nanofluids, in contrast, exhibited Nu of 51.3, 42.5, and 32.0 at identical entering conditions and with nanoparticle concentrations of 1, 2, and 3%, respectively. These represent decreases of 26.6%, 39.2%, and 54.2% relative to the base fluid. In the analytical model, the Nusselt number for Al
2O
3/60% EG nanofluids consistently exceeds the base fluid for concentrations between 1 and 3%, considering the entering conditions used in this test.
The data in
Figure 11 graphically illustrate the relationship between the liquid volumetric flow rate and the air coil heat rate. These data show that the nanofluids (1% Al
2O
3), at best, generate performance roughly equal to that of the base fluid at an equal flow rate and identical entering conditions. Generally, all the nanofluids tested produced lower heat transfer rates at equal liquid volumetric flow rates than the base fluid over the full range of flows tested. Previously developed analytical models predict that Al
2O
3/60% EG nanofluids with concentrations of 1% to 3% should generate heat rates 3–13% higher over a range of flows, considering the entering conditions tested here. Furthermore, the analytical model predicted that as the nanoparticle concentration in the heat transfer fluid increased, the heat transfer rate through the coil would increase at a given volumetric flow. Qualitatively, in this series of tests, as the nanoparticle concentration was increased, the heat rate of the coil decreased. At a volumetric flow of 0.125 L/s, the heat transfer rate was equal for the 60% EG and the 1% Al
2O
3/60% EG nanofluid. In contrast, the thermal outputs measured for the coils with 2% and 3% Al
2O
3/60% EG nanofluids were 5.7% and 14.6% lower than that for the 60% EG, respectively.
Figure 12 illustrates the relationship between the hydraulic pumping power
and the associated rate of air heat transfer while liquid volumetric flow rates were varied for all heat transfer fluids tested. The data show that for a given heat rate, the hydraulic power required to circulate the 1% Al
2O
3/60% EG nanofluid is 100% higher than that required for the 60% EG. For the 2% and 3% Al
2O
3/60% EG nanofluids, the hydraulic pumping power required was 129% and 371% higher than the 60% EG, respectively. The extremely high pumping is due to an extreme rise in viscosity caused by a high degree of agglomeration of particles.
The pressure loss measured through the coil tubing for the nanofluids and the 60% EG base fluid over a range of liquid volumetric flow rates is depicted in
Figure 13. As expected, the measured pressure losses for all of the nanofluids were significantly higher than those measured for the 60% EG at equal flows due to the higher viscosity of the nanofluids under these conditions. At a volumetric flow of 0.125 L/s, when circulating 1% Al
2O
3/60% EG, the observed pressure drop across the coil exceeds that of the 60% EG by 49%. The pressure drops measured while circulating the 2% and 3% Al
2O
3/60% EG exceeded that of the 60% EG by 48% and 64%, respectively.
These performance data were used to calculate, via the equation presented in
Section 3.2, the exergy consumed to generate a specific heat transfer rate, which offers a measure of the overall thermodynamic efficiency of the process and another means to compare the performance of nanofluids to the base fluid.
Figure 14 illustrates the relationship between the total exergy change for the liquid-to-air heat exchange process over a range of volumetric flow rates. The figure shows that, based on the measured performance, the total exergy utilization is higher for the 60% EG than for the nanofluids at equal flow. The experimental data qualitatively show the exergy consumed is generally higher for the 60% EG than the nanofluids. Still, since the heat rate associated with the flow rates deviates significantly at equal flow, with the base fluid heat rates generally higher, this comparison is of secondary importance to the comparison on a constant heat rate basis.
Figure 15 portrays the exergy change for the base fluid and the nanofluids as a function of the measured heat transfer rate. For example, the data reveal that the exergy change at a heat transfer rate of 4 kW (the rating of the tested air coil) is higher for the 60% EG than for the nanofluids. Once again, this comparison is based on the best-fit trendlines superimposed over the data sets. This indicates a higher exergy change required to achieve a given heat transfer rate for the 60% EG than for the nanofluid.
4.4. Challenge of Unstable Dispersion and Agglomeration
Based on previous theoretical analyses, the nanofluids tested here did not perform as expected. The thermal output of the heating coil circulating nanofluids was depressed relative to that of the coil circulating the base fluid, and the depression in output increased as the volumetric concentration increased. In contrast, based on system analysis, the peak heat output of the heating coil with 2% Al2O3/60% EG nanofluid was expected to exceed the output of the 60% EG by 7.3%, considering equal entering conditions at 0.125 L/s flow.
As stated earlier, multiple studies have tested nanofluids in heat exchange applications and have demonstrated superior performance to the associated base fluid. Based on a previous analysis, the authors’ hypothesis similarly predicted that the nanofluids would exhibit superior performance to the base fluid in the test apparatus. However, the experimental data do not support the hypothesis in this case. The result was unexpected because the nanofluids were produced using the same methods as in our past studies, resulting in nanofluids with thermal conductivities superior to those of their respective base fluids.
Potential explanations for the shortfall in performance are malfunctioning test instrumentation, damage or degradation of the heating coil, or poor fluid properties. A number of verifications can rule out the failure of equipment or instrumentation. These include physical checks of the equipment and, in the case of the thermistors, comparing the air thermistors’ readouts against the liquid thermistors under static conditions. Unfortunately, the authors had no readily available means of verifying the calibration of the air Venturi metering device (although the manufacturer validated the calibration device). The liquid flow meter was inspected on multiple occasions and was mechanically in good working order. Based on these field checks, the authors have determined that it is highly unlikely that the deviation from expected performance by the nanofluid is due to malfunctioning instrumentation or equipment.
Fouling of the heat transfer surfaces within the heating coil tube bank may also have occurred. However, no evidence of severe fouling was visible when the system was partially disassembled and visually inspected. Determining if the nanofluid properties were similar to those produced for earlier testing using similar methods is challenging; however, during the testing of the 3% Al2O3/60% EG nanofluid, two test runs were performed approximately 24 h apart. In the second test, the thermal performance of the nanofluid was significantly worse than that observed on the previous day. Specifically, the heat rate measured at a given flow rate was measurably lower on the second day versus the first. The observable degradation in the performance of the liquid indicates a degradation in the thermal properties of the liquid over time. None of the nanofluids prepared for the tests visibly changed in appearance, which could have been indicative that nanoparticles had settled out of suspension.
Earlier studies [
2,
3] have noted that pH can significantly impact nanoparticle suspension stability and have theorized that pH outside of an optimal range can alter nanoparticles’ zeta potential, leading to accelerated particle agglomeration. The nanoparticle dispersions used in this study were a few years old by the time they were used. Though the dispersions were stabilized with surfactants at the factory, these may have broken down, leading to degradation over time. Previous studies have reported that nanofluids containing larger agglomerated nanoparticles perform worse than finer nanoparticles. Settling of nanoparticles had been observed while the mother fluids were stored in the laboratory. It is difficult to ascertain after the fact if the nanoparticles’ surfactants and dispersants had broken down over time, causing agglomeration, thereby leading to the degradation of the thermophysical properties of the liquids. While experimenting on the freeze–thaw characteristics of nanofluids for their application in cold regions like Alaska, Sahoo et al. [
31] measured that nanoparticles’ average particle size grew by 51.2% in one case, due to agglomeration. Therefore, similar agglomerations might have occurred in the present sets of experiments on air coils with three concentrations, and the 3% concentration might have agglomerated the most. It should be noted that these experiments show a measurable degradation in the thermal performance of the nanofluids in this application as nanoparticle concentration increases. Furthermore, the 3% Al
2O
3/60% EG nanofluid exhibited a measurable decline in performance when tested successively within 24 h.
For these experiments with three nanofluids, other sources of thermal property degradation were identified, including contamination of the test loop liquid and degradation of dispersion properties over time. Contamination of the liquid can be caused by liquid trapped in the loop, which was mitigated by blowing out the loop with air to force any residue out. The authors attempted to verify the retention of purity of the nanofluids using a viscometer. This effort met with mixed results, as the viscosity readings did not agree closely with previous correlations derived from stable nanofluids.
Based on previous analysis, the test conditions employed for this study were quite favorable for the nanofluids. The viscosity penalty of the nanofluids relative to the base fluid at the higher entering temperatures was expected to be minimal. Additionally, at higher temperatures, the nanofluids’ higher thermal conductivity was expected to generate superior thermal performance in this test, with the largest advantage in heat rate for a given liquid flow rate and inlet temperatures expected for the 3% Al2O3/60% EG nanofluid. The fact that the nanofluid diminished the thermal performance of the heating coil and the degradation increased with the nanoparticle concentration is a significant finding. Therefore, this fluid type must be carefully considered to maintain ideal chemistry that ensures the suspension’s long-term stability and nanofluids’ enhanced performance.
A recent comprehensive computational investigation by Strandberg et al. [
32] proved that Al
2O
3, SiO
2, and CuO nanofluids of 1, 2, and 3% concentration could generate increasingly higher heat transfer coefficients than the base fluid under similar flow conditions. These computations were based on superior thermophysical properties prevailing throughout the life of the nanofluids. In nanofluids technology, that situation has not yet been attained. Therefore, there is a need for research to improve surfactants and dispersants for nanofluid stabilizing agents, which could preserve the superior thermal properties of nanofluids during their usage for years.
Despite the weakness of nanofluids found in our tests on heating coils in this research, it is encouraging that innovative studies continue internationally in this field. For example, Yu et al. [
33] demonstrated via molecular dynamics modeling simulations that hybrid nanofluids, e.g., Ag-Cu and Au-Cu, can yield higher thermal conductivity and better thermal performance than mono nanofluids like the Al
2O
3 used in our experiments, which have been investigated commonly. García-Rincón and Flores-Prieto [
34] examined the stability of nanofluids in flat-plate solar collectors and how to improve it. This will help harness green energy through a more efficient heat transfer fluid, which is already an important area of research nowadays. Gao and Li [
35] performed an experimental investigation on the effect of surfactants on the stability of nanoemulsions. Their methodology could be used to overcome the stability problem we faced with the Al
2O
3 nanofluid in our experiments. Through experimental and numerical investigations, Zakeri et al. [
36] presented encouraging results on recently adopted graphene oxide nanofluids. They found it can achieve up to 85% improvement in heat transfer coefficient compared to the base fluid. This is an impressive gain and certainly merits further research. Through CFD (computational fluid dynamics) analyses in a conical coil heat exchanger, using three hybrid nanoparticles (MgO-TiO
2, MOS
2-CuO, Ag-HEG) in water as a base fluid, Azaizi et al. [
37] summarized a comparison of the thermal performance of these nanofluids of various nanoparticle concentrations. All these recent studies would help in overcoming the drawbacks of nanofluids.
Nanofluids become unstable when the particle mass becomes large enough that the gravitational pull exceeds the buoyancy force and drag force, making the particle’s settling velocity higher than the upward component of the Brownian motion. The nanofluid is unstably dispersed in this condition, becoming microfluid, and loses all heat transfer benefits. The cause of particles growing larger is mutual attraction, which can be minimized via surface coating and adding liquids to the base fluid that prevent particles from attaching. When maintained within a desired range, the zeta potential, the electrical charge characteristic of these nanoparticles, ensures stable colloidal or nanoparticle dispersion. Another important characteristic of the nanofluid found in the research is that the pH value of a nanofluid is important in maintaining the stable dispersion of nanoparticles. For different nanofluids (e.g., Al2O3, CuO, SiO2, TiO2, etc.), optimum pH and zeta potential ranges can be determined in which the nanofluids behave the most efficiently in heat transfer. The nanofluids in heat exchangers should always be maintained to operate in those ranges of pH and zeta potential to obtain the gain promised by nanofluids.