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a r t i c l e i n f o a b s t r a c t
Article history: Phase change material (PCM) is used as a means of storing thermal energy. The method of PCM
Received 11 July 2016 containment in thermal energy storage (TES) systems is important as the material is in direct contact
Received in revised form with metal piping, plates and housing units which can be damaged if the material is corrosive. The
22 February 2017
compatibility of PCM with various materials for use in TES applications has been investigated using the
Accepted 27 February 2017
immersion corrosion method and suggestions to minimise their corrosive behaviour or to mitigate it by
using an alternative PCM have been presented and are described in the following paper. The metals and
plastics tested were copper, brass, aluminium, stainless steel, mild steel and Perspex. These were
Keywords:
Phase change material
immersed in ve different PCM, three fatty acids, a salt hydrate and Micronal for a period of 722 days.
Thermal energy storage Stainless steel was determined to be the most suitable of all the PCM investigated. Aluminium can be
Containment used with all fatty acids, however caution is advised as the maximum corrosion rate was found to be
Corrosion 12.4 m g/cm2year. Copper and brass can be encapsulated using fatty acid and again caution is advised as
Metal and plastic corrosion rates were found to be 22.15 g/cm2year and 1.67 g/cm2year, respectively.
2017 Elsevier Ltd. All rights reserved.
1. Introduction mild, boiler and austentic steels and the inuence of water and
other impurities was carried out and found LiCl-LiNo3-NaNO3 salt
Phase change materials (PCM) absorb thermal energy as latent mixtures lead to surface corrosion in all steels, NaCl-NaNO3 is
heat at a constant phase change temperature. PCM with a suitable compatible with all steels and KCl-LiCl are much more aggressive
phase transition temperature can be used to as a means of storing [17].
thermal energy for later use [1e3] or as a method of temperature Cabeza et al. carried out a series of short- [18], medium- [19] and
regulation of PV [4e7]. There has been considerable research on long- [20] term corrosion tests. The process involved immersing the
types of PCM, their applications and thermophysical properties metal sample in melted PCM in a test tube which remained in a
[8e12]. water bath for the duration of the experiment to ensure the PCM
PCM encapsulation can take the form of micro or macro remained in a liquid state. The short-term investigation involved
encapsulation [13e15]. With regard to macro-encapsulation, it is leaving the metal samples immersed in the following salt hydrates;
important the encapsulation material in the TES system is resistant zinc nitrate hexahydrate, sodium hydrogen phosphate dodecahy-
to corrosion by the PCM to ensure the system remains fully func- drate and calcium chloride hexahydrate with melting temperatures
tional for its lifetime. of 36 C, 35 C and 32 C respectively for a period of two weeks [18].
The availability of data on the corrosive nature of PCM was very The zinc nitrate hexahydrate emerged as a very corrosive material
limited until an investigation into the corrosion resistance of as aluminium and steel were highly corroded. Calcium chloride
metallic alloys to hydrated salts was carried out where stainless hexahydrate produced a pitting effect in aluminium and stainless
steel appeared to be the most corrosion resistant and aluminium steel. The samples continued to be immersed for 75 days [19].
the least [16]. Further investigation into the compatibility of high The metals previously mentioned were immersed in two PCMs
phase change temperature (160 C - 420 C) salt eutectics with TH29 and a chemical composition of MgCl2$6H20 for a period of
500 days in the long term corrosion tests [20]. As graphite can be
used as a method to increase the thermal conductivity of PCM, the
* Corresponding author. study immersed both the graphite and metal pieces in PCM.
E-mail addresses: brownema@tcd.ie (M.C. Browne), c13368026@mydit.ie
Aluminium and steel with either PCM are not recommended, brass
(E. Boyd), mccorms1@tcd.ie (S.J. McCormack).
http://dx.doi.org/10.1016/j.renene.2017.02.082
0960-1481/ 2017 Elsevier Ltd. All rights reserved.
556 M.C. Browne et al. / Renewable Energy 108 (2017) 555e568
and copper are recommended with both PCM and stainless steel is the corrosion rate. Finally, there has been no investigation into the
recommended for containment of PCM with caution. effect of PCM on Perspex a commonly used material which can be
Investigations into the compatibility of commercially available easily manipulated. The corrosive nature of PCM in TES systems is
PlusICE E17 and Climsel C18, two salt hydrates with melting tem- an important factor to be considered during system design as it will
peratures of 17 C and 18 C respectively, with an aluminium alloy impact on the lifetime of the system and thus, the economic ad-
and copper separately and aluminium in the presence of copper vantages of the system.
while immersed in an electrolyte [21]. The samples were immersed The methodology presented involves immersing ve materials,
in liquid PCM for 17 h. It was found copper samples experienced including metals and a plastic, in ve different PCMs for an
greatest mass loss varying between 0.8 and 0.145 g/(m2h) for extended period of time. The investigation records the rate of mass
ClimSel C18 and PlusICE E17, respectively. Aluminium showed loss of the metals and plastic at specied intervals over the course
pitting corrosion at a mass loss of 7 105 g/(m2h) while in contact of the experiment. In addition to this, a series of Scanning Electron
with ClimSel C18 with negligible mass loss when immersed in Microscopy (SEM) images were taken to assess the corrosion on a
PlusICE E17. For combined samples of aluminium and copper, no microscopic level.
mass loss occurred on the copper due to the cathodic protection but As the study presented is carried out under real time conditions,
the corrosion rate increased by a factor of 8 in Climsel 18 compared it presents a more detailed account of the natural corrosion process
to aluminium alone [21]. Garca-Romero, Delgado, Urresti, Martn of material samples immersed in PCM compared to accelerated
and Sala [22] presented the corrosion behaviour of four aluminium methods. The paper shows the calculation of the rate of corrosion of
alloys (EN AW 2024, 3003, 6063 and 1050) in the commercial salt each sample by the individual PCM. This provides an insight into
hydrate Glaubers salt (Na2SO4$10 H20) which has a melting point of the extent of the corrosive nature of PCM and can be used to ensure
32 C. Samples were fully and partially immersed in the PCM and the optimum encapsulation material is chosen during system
experiments were conducted for a period of up to 90 days. It was design. Furthermore, SEM imaging can be used for a greater insight
found the aluminium alloy 2024 was not compatible with this into the initial stages of corrosion which are not initially visible to
specic salt hydrate, however, 3003, 6063 and 1050 were shown to the naked eye.
be fully compatible.
An investigation into the corrosion resistance of metal samples, 2. Materials and methodology
stainless steel, carbon steel, aluminium and copper to fatty acids
stearic, palmitic, myristic and lauric acid with melting tempera- This section describes the material samples assessed for corro-
tures between 40 C - 63 C [23]. Following 910 thermal cycles of sion resistance, in addition to the PCM investigated. The method-
being fully immersed in each PCM, the metal samples were ology of the experiment is presented to show the approach
removed and a gravimetric analysis carried out. The highest undertaken. Finally, a brief description of scanning electron mi-
corrosion rates calculated were 3.4 102 and 4.9 102 mg/cm2 croscopy is given as images of the samples were taken on specic
for carbon steel in contact with myristic acid and copper in contact days throughout the experiment to assess the level of corrosion at
with stearic acid. Stainless steel with a chromium oxide layer and an increased magnication.
aluminium with an aluminium oxide layer were found to be
compatible with fatty acids. 2.1. Material samples
An investigation into the compatibility of four organic and one
salt hydrate PCM (namely a molecular alloy C16-C18, RT20, RT26, Five materials that are commonly used in TES system designs
RT25 and TH24) and plastics (high density polyethylene, low den- and construction [5,29e31] were tested in the experiment. The
sity polyethylene, polyethylene terephthalate and polypropylene) metals were aluminium, brass, copper, stainless steel, steel and the
was carried out [24]. A furnace was used to cycle the plastic bottles plastic used was Perspex. The chemical compositions of the mate-
to increase the rate of phase change. LSPE was discarded as an rials tested are presented in Table 1 using a Tescan Mira Scanning
encapsulation material due to the mass variations and large de- Electron Microscope. The samples were cut from larger pieces of
formations caused by the PCM. Polyethylene terephthalate and materials and each had dimensions of 50 mm 14 mm and a depth
polypropylene were shown to be the best encapsulation material of of 2 mm.
the organic PCM and high density polyethylene for inorganic PCM.
Polypropylene, polyethylene terephthalate and low density poly- 2.2. Phase change material (PCM) samples
ethylene are not recommended for using with TH24.
Further immersion corrosion tests have been carried out for a Fatty acids are an organic PCM and have many superior prop-
period of 84 days on aluminium, stainless steel, carbon steel and erties including high heat capacity, congruent melting, little or no
with salt hydrates, salt hydrate eutectics and fatty acid eutectics supercooling, non-toxic, good thermal and chemical stability, low
[25e27]. The results suggest that stainless is recommended for use cost, non-ammable and small volume change [32e34]. They are
with any of the PCM studied and all other metals would either be known to have high melting temperatures which are outside the
recommended with caution or not be recommended at all. Fatty range of thermal energy storage applications [35]. To overcome
acid eutectic of capric:palmitic (75.2:24.8%) show that copper is the this, a eutectic mixture of fatty acids is two or more fatty acids
only material tested which is not suitable for containment of the combined to form a binary fatty acid with a lower phase change
PCM. However, these tests were carried out for a short period of temperature and feature the same stability of a single component.
time and further analysis should be carried out to draw accurate The advantage of fatty acid eutectics is the ability to gain a lower
conclusions. Oro , Barreneche, Farid and Cabeza [28] has also melting temperature with all the material advantages of a fatty acid
investigated the compatibility of metal and polymers with PCM by varying the mass ratio of the mixed fatty acids [35,36]. Capric
with lower phase change temperatures (22 C to 16 C). acid and two fatty acid eutectics, capric:palmitic and capric:lauric
There has been no research carried out on eutectic fatty acids, acid have been investigated. Capric:palmitic acid is a mixture of
particularly capric, palmitic and lauric acid which have often been 75% capric and 25% palmitic by weight and capric:lauric acid is a
used in thermal energy storage systems. The phase change process mixture of 45% capric and 55% lauric acid.
has been accelerated using furnaces and thermal cycling however, Inorganic salt hydrates consist of salt and water which combine
due to the reduced time immersed in PCM may potentially affect in a crystalline matrix when the material solidies. Different salts
M.C. Browne et al. / Renewable Energy 108 (2017) 555e568 557
Table 1
Composition of metals and plastic samples.
Material
are used in combination with water to alter the phase change 2.3.2. Corrosion test of metal and plastic materials
temperature. As the crystal is heated it melts, releasing the water of Following sample preparation, each material sample was placed
crystallisation and allowing the salt to dissolve in the water [37]. in a test tube and immersed in PCM. The samples were completely
They are attractive materials for TES due to their high thermal covered in PCM and the test tube was sealed to avoid ingress of
conductivity [38] and as a result the commercially available salt moisture and water from the water bath. There was no attempt
hydrate SP22 was used in the investigation. made to avoid contact with oxygen in the air so as to match as
Micronal is a material designed for temperature regulation closely as possible the expected on-site conditions within a thermal
applications and its performance has been investigated within storage unit. The test tubes were then placed in a water bath at a
buildings [39]. The PCM wax mixture, classied as organic parafn, constant temperature of 45 C to ensure all PCMs remained in a
is contained in small vessels (particle diameter 5 mm) with the core liquid phase and were not stirred.
PCM and a hard covering material [40].
A full list of PCM investigated is presented in Table 2 along with 2.3.3. Sample weighing
thermophysical properties. The phase change range and heat of The samples were then cleaned with acetone to remove any
fusion have been found using the differential scanning characteri- impurities from the material surface. Each material sample was
sation technique and are in agreement with previously reported removed from the PCM every 7 days, cleaned with tap water to
literature [6,8,41]. remove any excess PCM and then weighed using a Kerns PCB to the
nearest 0.01 g. This process was repeated every 7 days for 722 days
in total. In addition to this the samples were visually evaluated for
2.3. Methodology bubbles, precipitates, surface changes and pitting.
The methodology used in this study was based on the Standard 2.3.4. Corrosion assessment
Practice, Cleaning, and Evaluating Corrosion Test Specimens (ASTM The evaluation of the corrosion results involved completing a
G1-01) and has been applied to corrosion investigations of PCM and gravimetric analysis which consisted of the mass loss of the sample
metals [18e20,25]. The process was divided into four steps. with respect to the initial mass as in Eq. (1).
Dm mt0 mt (1)
2
2.3.1. Preparation of the sample The corrosion rate (CR) (mg/cm year) of the samples was then
The preparations of the samples required cutting them from determined by taking into account the mass loss (Dm), the area of
larger pieces of materials to approximately 50 mm 14 mm and a the material (A) and the experimental time (t0 - t) and applying
depth of 2 mm. The samples were then cleaned with acetone to them in Eq. (2).
remove any impurities from the material surface. Prior to the
Dm
experiment the samples were weighed using weighing scales (Kern CR (2)
scales accuracy of 0.01 g) and the values were recorded. A$t0 t
Table 2
List of materials and PCM used in corrosion experiments.
SEM is a scanning electron microscope that produces images by Fig. 1. Material mass loss due to immersion in capric acid.
scanning it with a focused beam of electrons. The electrons interact
with atoms in the sample material, producing various signals that
can be detected and that contain information about the samples
surface topography. To ensure the samples were fully visually
examined a Tescan MIRA scanning electron microscope (SEM) was
used to take images on Day 1, Day 35, Day 200 and Day 500. SEM
allowed for images to be taken at magnications of 200, 3000
and 6000 which allowed for the inspection of initial signs of
corrosion not visible to the naked eye.
Table 3
Guide for corrosion weight loss used in the industry.
Fig. 7. Copper, brass and stainless steel samples in (a) capric acid (b) capric:palmitic acid (c) capric:lauric acid.
Fig. 8. Material mass loss due to immersion in SP22. Fig. 11. Corrosion rate during immersion tests of material samples with Micronal.
than any other material tested, as shown in Fig. 10. The mass loss of The samples were investigated under a microscope for signs of
mild steel reached a value of approximately 0.4 g compared to the corrosion on Days 1, 25, 200 and 540 using magnications of 200,
corrosion weight loss of all other material samples being less than 3000 and 6000. However, due to the transparent nature of
0.04 g. Perspex this material could not be used in the SEM imaging.
The evolution of corrosion rate of materials immersed in Stainless steel has not been affected by the PCM in any immersion
Micronal is presented in Fig. 11. Initially, the mild steel corrosion tests and as a result there is no presentation of images of stainless
steel. From photographic images, the rate of corrosion can be
visually observed as the size of the pitting in some samples in-
creases with the length of time it was immersed in the PCM.
pitting (as seen in Fig. 13) although there still some evidence of the surface can be seen to be full of large areas of pitting (Fig. 17c) by
surface layer being intact due to the vertical indents which is ex- Day 540. The corrosion shown in the images reect the mass loss
pected as the mass loss of 0.29 g is less than that of copper and found over the course of the immersion corrosion tests. The initial
capric acid. mass of 10.19 g was reduced by 0.05 g by Day 200 and by 0.19 g on
Aluminium had an initial mass of 3.13 g and can be seen to avoid Day 540.
excessive corrosion up to Day 200 as the horizontal textured lines The aluminium sample immersed in capric:palmitic acid can be
are evident this is also shown in the mass loss of 0.01 g (Fig. 14b). seen in Fig. 18. The sample withstands the corrosive effect of the
The pitting is clearly seen in the images taken on Day 540 Fig. 14c material until approximately 200 days when pitting can be seen in
when the corrosion got progressively worse as the mass loss was image (b) along with some of the intact surface material of the
0.2 g. sample which would reect a mass loss of 0.01 g. By Day 540 the
The mass loss and corrosion rate of mild steel in capric acid surface has been badly corroded as no vertical lines can be seen and
which was 0.83 g and 0.031 g/cm2year on Day 722 showed that the this is shown in mass loss of 0.27 g, an 8.6% loss on the initial mass.
material was adversely affected by the PCM. The images shown in Mild steel can be seen to be corroded from early on in the
Fig. 15 reect this and although there is no deep pitting, the layer on experiment, as on Day 25 small areas of pitting are obvious which
the surface of the material can be seen to change over time as it is was also seen in the mass loss of 0.1 g (Fig. 19) and the surface of the
being worn away by the corrosive PCM. sample can be seen to have vast areas of pitting (Fig. 19c) by Day
540 which showed a mass loss of 0.85 g, 9.1% of the total initial
mass.
3.2.2. Capric:palmitic acid
Capric:palmitic has been shown to corrode metals when
considering the mass loss and corrosion rate results of the gravi- 3.2.3. Capric:lauric acid
metric study. Capric:lauric acid showed the same corrosion patterns to that of
Copper had an initial mass of 10.65 g and can be seen to be the previous two fatty acid PCM. Copper and brass samples, as
affected by the corrosive nature of capric:palmitic acid by Day 200 presented in Figs. 20 and 21; appear to have signs of pitting by Day
the mass had reduced by 0.07 g. The vertical lines are barely visible 25 which got increasingly worse as the experiment progressed.
and vast areas of pitting can be seen to be forming as shown in By Day 540 it can be seen the surface of the samples are
Fig. 16b. Day 540 shows the surface of the sample has been completely corroded. The images showed the corrosion process
corroded by the PCM Fig. 16c which was a result from the corrosion whereby there was a mass loss of 0.01 g on Day 25 by both mate-
of the surface and a mass loss of 0.37 g. rials. Copper has shown to be more susceptible to corrosion by
Similar to the copper results, brass immersed in capric:palmitic capric:lauric acid than that of brass as the mass loss was shown to
acid shows areas of pitting after Day 200 (Fig. 17b) and the entire be 0.43 g by Day 540 for copper and 0.26 g for brass which is
Fig. 13. Brass immersed in capric acid on (a) Day 1 6000 magnication (b) Day 200 6000 magnication (c) Day 540 6000 magnication.
562 M.C. Browne et al. / Renewable Energy 108 (2017) 555e568
Fig. 15. Mild steel immersed in capric acid on (a) Day 1 6000 magnication (b) Day 25 6000 magnication (c) Day 540 6000 magnication.
reected in the images taken using SEM. Fig. 22 shows aluminium of the material almost entirely corroded where the mass loss was
immersed in capric:lauric acid, the images show the process of found to be 0.71 g.
corrosion had started by Day 200 as one large area of pitting can be
seen in Fig. 22b. By Day 540 the entire surface of the metal has been
completely broken down which is seen in Fig. 22c and reected in 3.2.4. Salt hydrate SP22
the mass loss results as 3.2% of the initial weight had been corroded SP22 has been shown to result in severe corrosion on aluminium
by this stage of the experiment. in the gravimetric analysis and minor corrosion on the remainder of
The microscopic evaluation of mild steel immersed in capri- the samples. It is interesting to note that corrosion may not be
c:lauric acid is presented in Fig. 23. The grain boundaries of mild evident in the gravimetric analysis but the initial stages of corrosion
steel can be seen in (b) which indicates the weak points of the can be seen using SEM imaging. An example of this is copper
material that are most susceptible to corrosion by the fatty acid immersed in SP22 as pitting can be seen in Fig. 24c and had a mass
eutectic and have reported a mass loss of 0.18 g by Day 200. The loss of 0.02 g by Day 540. This is due to the large magnication of
material is seen to be further corroded by Day 540 with the surface the SEM images which showed the initial stages of corrosion which
were not large enough to be determined by the weighing scale.
564 M.C. Browne et al. / Renewable Energy 108 (2017) 555e568
Fig. 21. Brass immersed in capric:lauric acid on (a) Day 1 6000 magnication (b) Day 25 6000 magnication (c) Day 540 3000 magnication.
Images of aluminium which has been immersed in SP22 are corrosion can be seen in Figs. 26 and 27 for these materials. Small
presented in Fig. 25. The aggressive corrosion is evident as pitting pockets of pitting in the images taken on Day 540 suggest given
can be seen in (b) after only 25 days. time the material will further corrode which is also shown by the
The grain boundaries can be seen to be depleted in (c) which has progressive mass loss of 0.01 g on Day 200 and 0.04 g on Day 540
been taken on Day 540 when mass loss of 0.01 g was reported. The experienced by both materials.
delay in mass can be explained by the initial low mass of the ma- Aluminium was extensively corroded from exposure to Micro-
terial sample, 3.14 g. Such extensive corrosion can compromise the nal. Numerous small areas of pitting can be seen in Fig. 28b which
mechanical properties of materials. increase and grow in size by Day 540 this reects the reported mass
loss of 0.01 g (Fig. 28c). It is worth noting this image is taken at a
3.2.5. Micronal magnication of 200 to emphasis the aggressive nature of
Although, copper and brass immersed in Micronal did not Micronal on aluminium.
show signs of corrosion in the gravimetric analysis, early stage
M.C. Browne et al. / Renewable Energy 108 (2017) 555e568 565
3.3. Evaluation and recommendation up to 22.15 mg/cm2year compared to the corrosion rate of 1.67 mg/
cm2year of copper in Micronal. Aluminium is affected by fatty
The nal results of the mass loss and corrosion rate of each acids which have shown corrosion rates of up to 12.04 mg/cm2year
material immersed in PCM after 722 days are summarised in although this is less than the corrosion rate of copper, brass and
Table 4. Overall, it can be seen that mild steel is an unlikely mild steel which have shown corrosion rates of up to 37.58 mg/
candidate for encapsulation of PCM particularly fatty acids and cm2year in fatty acids. The material loss of stainless steel and
Micronal which was shown to have the highest mass loss of Perspex is negligible and it can be assumed these materials are
0.88 ge1.09 g and 0.4 g for fatty acids and Micronal, respectively. compatible for use with PCM.
Aluminium showed the highest mass loss of all materials immersed The corrosion rate was measured in g/cm2year which has been
in SP22 of 1.17 g; the salt hydrate was shown to aggressively attack changed to mg/cm2year to be used in combination with the
the passivation layer it produces for self-protection causing further corrosion weight loss standard guide. The document is used in in-
corrosion of the material. Brass and copper are seen to be corroded dustry to dene the degree of corrosion considered excessive and
by the fatty acids more than the other PCM with corrosion rates of gives an indication of the period of recommended use. The results
566 M.C. Browne et al. / Renewable Energy 108 (2017) 555e568
Fig. 27. Brass immersed in Micronal on (a) Day 25 3000 magnication (b) Day 200 3000 magnication (c) Day 540 3000 magnication.
Table 4
Corrosion results obtained by gravimetric analysis after 722 days.
Metal Capric acid Capric: palmitic acid Capric: lauric acid SP22 Micronal
sample
Mass loss Corrosion rate (mg/ Mass loss Corrosion rate (mg/ Mass loss Corrosion rate (mg/ Mass loss Corrosion rate (mg/ Mass loss Corrosion rate (mg/
(g) cm2yr) (g) cm2yr) (g) cm2yr) (g) cm2yr) (g) cm2yr)
Copper 0.65 22.15 0.48 16.39 0.5 17.4 0.02 0.68 0.05 1.67
Brass 0.39 13.57 0.27 9.31 0.32 10.9 0.02 0.7 0.03 1.02
Aluminium 0.2 7.08 0.34 12.04 0.12 4.25 1.17 41.45 0.01 0.33
Stainless 0.01 0.37 0 0 0 0 0 0.0 0 0
steel
Mild steel 0.93 31.07 1.09 37.58 0.88 30.34 0.08 2.75 0.4 14.72
Perspex 0 0 0 0 0 0 0.02 0.63 0 0
of the suitability of tested encasement material-PCM pairs are overall economic feasibility of the system when considering the
presented in Table 5. The metallographic investigation is also taken suitability of a PCM - encasement material pair as it as suggests the
into account when making the decision. container will not have to be replaced during the lifetime of the
Samples have been categorised into recommended, not rec- system. Ideally, a material with a recommended relationship with a
ommended and caution. Recommended suggests the material-PCM PCM would be the primary choice for integration into a PV/T/PCM
pair is compatible for long term service as the corrosion rate was system. However, other factors such as thermal conductivity and
less than 0.3 mg/cm2yr. A Recommended result improves the implications of manufacture should be also considered.
Table 5
Suitability of material e PCM pairs studied for use in a TES system.
Capric acid Capric: palmitic acid Capric: lauric acid SP22 Micronal
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