Giro Paloma2016

Renewable and Sustainable Energy Reviews 53 (2016) 1059–1075
Contents lists available at ScienceDirect
Renewable and Sustainable Energy Reviews

journal homepage: www.elsevier.com/locate/rser
Types, methods, techniques, and applications for microencapsulated

phase change materials (MPCM): A review
Jessica Giro-Paloma a, Mònica Martínez a, Luisa F. Cabeza b,1, A. Inés Fernández a,n
a
Departament de Ciència dels Materials i Enginyeria Metal lúrgica, Universitat de Barcelona, Martí i Franqués 1-11, 08028 Barcelona, Spain
b
GREA Innovació Concurrent, Edifici CREA, Universitat de Lleida, C/ Pere de Cabrera s/n, 25001 Lleida, Spain
art ic l e i nf o a b s t r a c t
Article history: Phase change materials (PCM) can be employed in many fields because of their capacity to absorb and
Received 1 August 2014 release energy when it is necessary. Nowadays, the number of studies about these materials is increasing
Received in revised form because of their benefits in energy systems. This paper reviews the previous researches and develop-
8 June 2015
ments on microencapsulated phase change materials (MPCM) in thermal energy storage (TES) systems,
Accepted 18 September 2015
focusing on the different methods of encapsulations and also the different applications of these mate-
Available online 10 November 2015
rials. This review aims to be a useful guide for the researchers in this area, because it explains the dif-
Keywords: ferent types of phase change core materials, the different shells, the methods to microencapsulate these
Phase change material PCM, the most used techniques to characterize these microencapsulated phase change materials, and a
Microencapsulated phase change material
revision of the main applications.
Thermal energy storage
& 2015 Elsevier Ltd. All rights reserved.
Contents
1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1060
2. Types of phase change materials (PCM) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1061
2.1. Organic PCM . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1061
2.1.1. Paraffin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1061
2.1.2. Fatty acids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1062
2.2. Inorganic PCM . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1062
2.2.1. Salt hydrates . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1062
2.2.2. Salts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1062
2.2.3. Metals. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1062
2.3. Eutectics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1062
3. Types of shell. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1062
4. Types of microencapsulated phase change materials (MPCM) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1062
5. Methods to encapsulate PCM . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1063
5.1. Chemical methodology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1063
5.1.1. Suspension polymerization . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1063
5.1.2. Dispersion polymerization. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1064
5.1.3. Emulsion polymerization. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1064
5.1.4. In situ polymerization . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1064
5.1.5. Interfacial polymerization . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1065
5.2. Physico-chemical methodology. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1065
5.2.1. Coacervation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1065
5.2.2. Sol–gel encapsulation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1066
5.2.3. Supercritical CO2-assisted . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1066
5.3. Physico-mechanical methodology. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1067
n
Corresponding author. Tel.: þ 34 934021316; fax: þ 34 93 4035438.
E-mail addresses: [email protected] (J. Giro-Paloma), [email protected] (M. Martínez), [email protected] (L.F. Cabeza),
[email protected] (A.I. Fernández).
1
Tel.: þ34 973003576; fax: þ 34 973003575.
http://dx.doi.org/10.1016/j.rser.2015.09.040
1364-0321/& 2015 Elsevier Ltd. All rights reserved.
1060 J. Giro-Paloma et al. / Renewable and Sustainable Energy Reviews 53 (2016) 1059–1075
5.3.1. Spray-drying . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1067

5.3.2. Electrostatic encapsulation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1067
5.3.3. One-step method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1067
6. Phase Change Slurries . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1067
7. Characterization of MPCM. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1067
7.1. Experimental characterization techniques reported in the study of MPCM . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1067
7.1.1. Particle size distribution (PSD) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1067
7.1.2. Optical microscopy (OM) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1068
7.1.3. Scanning electron microscopy (SEM) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1068
7.1.4. Transmission electron microscopy (TEM) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1068
7.1.5. X-Ray diffraction (XRD) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1068
7.1.6. Wide angle X-ray scattering (WAXS) and low angle laser light scattering (LLALS) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1068
7.1.7. Fourier transformed infrared spectroscopy (FT-IR). . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1068
7.1.8. Differential scanning calorimeter (DSC) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1069
7.1.9. Thermogravimetrical analysis (TGA) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1069
7.1.10. Atomic force microscopy (AFM) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1069
7.1.11. Emission of volatile organic compounds . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1069
7.2. Properties to analyze . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1069
7.2.1. Flammability . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1069
7.2.2. Viscosity measurement, density, and conductivity. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1069
7.2.3. Cycling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1070
8. MPCM applications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1070
9. Conclusions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1071
Acknowledgments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1071
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1071
1. Introduction comfort can be used, which is around 20 7̄ C. One of these appli-

cations for PCM is climatization [10], which has different uses, for
Phase change materials (PCM) are well known in thermal example in solar cooling, as the study of Gil et al. [11] shows.
energy storage (TES) applications [1–3]. PCMs are used to store Besides, inside the refrigeration area, food conservation [12,13] can
energy when it is available, absorbing it and releasing it when be included. Oró et al. [14] studied the effect of the PCM intro-
needed. The most important requirements to be a good PCM may duction outer a freezer, improving the quality in the ice cream. The
be divided in physical, chemical or economical requirements: container drinks can also incorporate these type of materials to
store energy, and release it when the systems needed, for example,
Physical requirements: suitable phase change temperature, the chilly bins studied by Oró et al. [15] to enhance the thermal
complete reversible freeze/melt cycle, large change in enthalpy performance. Also, it is possible to use phase change materials in
(ΔH), large specific heat capacity (Cp), large thermal con- cold storage needs, as Oró et al. [16] evaluate, studying the com-
ductivity (k), and little subcooling. patibility of PCM with metallic materials, but a common problem
Chemical requirements: small volume pressure, low vapor in PCM cooling applications is the subcooling, which happens
pressure, good compatibility with other materials, chemical
when a material is cooled and the crystallization does not start
stability, physical stability, and non-toxicity.
below the freezing temperature [17].
Economical requirements: low price, recyclable and abundant.
Another very significant application of PCM is the one in the
building sector [18], in passive applications like floors [19], walls
PCM are used in several applications, due to the research done
[20–23] (for example conventional and alveolar brick [24]), and
last 40 years in this field. It had been published a total of 10,892
documents in TES field for the last 10 years (January 2005–April 90
2015) [4]. Taking into account TES subject, if it is emphasized in 81
PCM field, 2319 documents can be counted. Following the same 80
bibliographic search, but deepening and specializing the topic, the
70
representation for the search in microencapsulated phase change 63 64
material (MPCM) in TES field, is shown in Fig. 1, with 449 docu- 60
related MPCM in
ments for the last 10 years (January 2005–April 2015).

Nº documents
49 49
TES field
These 449 documents related to MPCM were published in 50

different subjects inside TES area. The most part were from Engi-
40 37
neering (46.1%), Materials Science (30.1%), and Energy (28.1%)
journals, as Fig. 2a illustrates. The studies connected with this 29
30
thematic were produced in different kind of publications, such as 23
19 18
articles (70.2%), conference papers (24.3%), and reviews (2.9%), as 20 17
examples shown in Fig. 2b. Up to date, there are no reviews
10
on MPCM.
From these figures the study of PCM and MPCM is a topic that 0
generates more interest every year. These materials can be applied 2015 2014 2013 2012 2011 2010 2009 2008 2007 2006 2005
in textiles [5,6], buildings [7–9], packaging, food, medical thera- Year
pies, etc. PCM have been considered for TES in buildings since Fig. 1. Representation of the publications total number related to MPCM in TES
1980, and only the PCM with a phase transition close to the human field between 2005 and 2015.
J. Giro-Paloma et al. / Renewable and Sustainable Energy Reviews 53 (2016) 1059–1075 1061
Other (7.1 %) Book chapter (0.2 %)

Biochemistry (1.8 %) Article in Press (1.1 %)
Business, Management (2.2 %) Engineering (46.1 %)
Computer Science (2.7 %) Conference Review (1.3 %)
Environmental Science (14.5 %) Review (2.9 %)
Chemistry (14.5 %)
Conference Paper (24.3 %)
Physics and Astronomy (15.1 %)
Chemical Engineering (23.8 %) Materials Science (30.1 %)

Article (70.2 %)
Energy (28.1 %)
Fig. 2. (a) Documents by subjects for MPCM in TES field; (b) Documents by type for MPCM materials in TES field.
ceiling studies. There is another case, which is in active systems in which will be used in a system as a good material to store energy
domestic applications as heating [25] and hot water [26–29]. is chosen, it is very important modeling the system with the fin-
Since PCM undergo the solid–liquid states, they need to be ality to know how it will perform [40].
encapsulated for their inclusion in the final system. Due to the Microencapsulation has been studied widely by many
leakage in the liquid state when mixing the PCM with other researchers, but the literature is scattered. Therefore, this paper
materials, such as building construction materials [30], and presents a review, which includes the different types of PCM that
because of the corrosion and the thermal reliability, the possibility can be microencapsulated, the different shell materials used, the
to make a polymeric container for PCM, in small vessels, using the way to microencapsulate these PCM, and finally the most used
encapsulation technology and producing capsules calling them techniques to characterize these MPCM with the idea to organize
encapsulated phase change material for energy storage [31] has such literature and help researchers to use it as a guide in their
been investigated. Encapsulation techniques vary from macro- future work. At the end of the review, the most important appli-
encapsulation in slabs, panels, etc. to microencapsulation [32,33]. cations where MPCM are used are summarized. The future direc-
When the sizes of these capsules are micrometers, these are called tions of research and development on microencapsulated phase
microencapsulated phase change material (MPCM), which con- change materials will focus on the improvement of characteriza-
sisted on a polymeric shell and a core made of the storage mate- tion methodology for such complex materials, and deeply studying
rial. The microencapsulation is a process of enclosing micron-sized other relevant properties as the volatile organic compounds
particles of solids or droplets of liquids or gases in an inert shell, spread by MPCM, as well as their fire behavior.
which in turn isolates and protects them from the external
environment. The captivity of waxes into the microcapsules allows
to increase the heat transfer [3] and to control de volume changes 2. Types of phase change materials (PCM)
when the phase change is happening. Microencapsulation meth-
odology for PCM still needs to be improved because the micro- In microencapsulation, the core material is defined as the
capsules can break easily when they collide with other micro- specific material to be coated and can be in liquid or solid state
capsules when they are used in active systems. Moreover, the shell depending on the temperature. The composition of the solid core
has to be strong enough to sustain the stresses that are generated can be a single solid substance or a mixture of active constituents,
due to the volumetric changes during the phase change process of stabilizers, diluents, excipients and release-rate retardants or
the PCM. accelerators [41,42]. There are three type of PCM: organic, inor-
There are three requirements for the microencapsulation pro- ganic and eutectic PCM. The most important property to take into
cess: the formation of the shell around the desired PCM, guaran- account in a material to be used as a PCM is that it must have high
teeing that there is not leakage and ensuring that no impurities are thermal energy storage capacity, and in general, inorganic have it
included in the system core/shell MPCM. Besides, the thickness of higher than organics, but there are some other subjects to take
the coating material has to assess the effectiveness of the encap- into account for choosing these materials. Cabeza et al. [43] listed
sulated PCM. For this reason, the MPCM have to be highly resistant in their review many PCM specifying their type, melting tem-
to mechanical and thermal stresses. perature, heat of fusion, thermal conductivity, density, and their
Two studies by Jamekhorshid et al. [34] and Sukhorukov et al. source.
[35] explain that the size of the MPCM is very significant, because
MPCM are more stable in the nanosize than in the microsize. They 2.1. Organic PCM
observed less mechanical deformation in 10 nm MPCM in size
than in 10 μm. To avoid the breakage of the microcapsules, it is This type of PCM is further described as paraffinic and non-
important to take into account the whole system we are using paraffinic. The principal advantages are their chemical and ther-
(shell/core). Moreover, the compatibility of plastics with PCM is a mal stability, they are non-corrosive, recyclable and they have no
key point as Castellón et al. [36] evaluated, concluding that LDPE subcooling. On the other hand, the disadvantages of using organic
and PP show worst behavior compared with HDPE to encapsulate PCM are their flammability, their low thermal conductivity and a
PCM. Hardness and Young0 s Modulus of different polymers were phase change enthalpy lower than other type of PCM. The most
evaluated by Giro-Paloma et al. [37], because in passive systems used ones are paraffin and fatty acids:
case [38], the main problem of the leakage is the compression of
this microcapsules inside the wall in a building [39]. 2.1.1. Paraffin
As Kuznik et al. [23] studied, there are three relevant char- This chemical is produced as a by-product of petroleum refin-
acteristics to evaluate for the quality of the MPCM: the mean ery. It consists of carbon and hydrogen atoms joined with single
diameter, the thickness of the shell, and the mass percentage of bonds with the general formula: CnH2n þ 2, where n is the number
PCM compared to the total mass of the capsule. Once the PCM of carbons (C). When n is between 1 and 4 C atoms the material is
Table 1
Manufacturers of MPCMs.
Trademark name PCM Shell material PSD Application
Cristopia Eutectic salts Polyolefin 77 mm Industrial refrigeration, building, conditioning

ClimSel/climator Sodium acetate, sodium sulfate – – Medicine transportation, clothing, air-conditioning,
electronic cooling, fire protection
Rubitherm Paraffin, salt hydrate in granulate, pow- Plastic – Storage and transport food, medical equipments, storage
der and compounds forms materials for textile
TM
Latest /TEAP Energy Glauber’s salt, soda ash, sodium acetate, Polyethylene 25.4 mm Hot pads and solar heating telecom enclosure, back-up
and paraffin wax air-conditioning, cold storage
PCM Products Ltd. Eutectics, salt hydrates, organic materi- Rubber, HDPE plastic 40 mm Space International space station, automotive passive
als, and high temperature salts cooling, solar heating and heat recovery
MPCM Microtek Laboratories Paraffin Polymer 17–20 μm Active wear clothing, woven and non-woven textiles,
Inc. building materials, packaging, and electronics
s s
Micronal /BASF Paraffin wax Polymer 5 μm Building conditioning, surface cooling
Aegis Inorganic salts High density 75 mm Cold storage, boilers, solar water heaters, transport of
polyethylene blood, frozen food, fruits and vegetables
gaseous; between 5 and 17 C is liquid, and for more than 17 C is 2.2.3. Metals
solid. It is considered a paraffin wax when the C is in the range This subcategory of inorganic PCM includes the low melting
of 20–40. metals and metal eutectics. They are good candidates to take into
account for elevate temperature of phase change, when the
2.1.2. Fatty acids volume is a consideration in the system, because of their high heat
It is a carboxylic acid with a long hydrocarbon chain of carbon of fusion per unit volume. This type of PCM has high thermal
(from 10 to 30) and hydrogen atoms with a general formula conductivity, low specific heat, and low vapor pressure.
CH3(CH2)2nCOOH. It has the carboxyl group (COOH) at the end of
the chain and due to the protection of this group, fatty acids based 2.3. Eutectics
PCMs are non-toxic, with low corrosion activity, and chemically
The eutectics are a combination of chemical compounds or
and thermally stable. Moreover, they can be found in natural
elements that has a single chemical composition and solidifies at a
products, not being a fossil fuel derivative. The fatty acids can be
lower temperature than any other composition obtained from the
saturated or unsaturated, with one or more double bounds.
same components. The combinations can be organic–organic,
Unsaturated fatty acids have lower melting points due to the inorganic–inorganic, or inorganic–organic [45]. There are numer-
molecular structure that allows closer molecular interactions. ous eutectic mixtures suitable to be used as PCM, and they are
Moreover, unsaturated fatty acids can exist in the cis and trans preferred in cooling applications.
configuration having the intermolecular interactions weaker than
in saturated ones. Besides, different fatty acids can be mixed to
design PCMs with different melting temperatures. There is a study 3. Types of shell
of Suppes et al. [44] where the possibility to use natural fatty acid
mixtures as high performance PCM is demonstrated. There are over 50 different polymers known that can be used as
wall materials in microencapsulation; both natural and synthetic
polymers controlling release under specific conditions. The shell
2.2. Inorganic PCM coating materials have to have some properties or requirements.
The polymer should be capable of forming a thin film that it must
They are classified as salt hydrates, salts, and metals. This type be cohesive with the core material, being tasteless, pliable, and
of materials has fewer advantages than organics. The pro is that stable. It should be chemically compatible and non-reactive with
they have higher phase change enthalpy, but the corrosion, sub- the core material, and also soluble in an aqueous media or solvent.
cooling, phase segregation, lack of thermal stability, and phase Moreover, it should provide the desired coating properties such as
separation are the most important cons. strength, flexible, impermeable, optical properties, and stability.
The film thickness can be varied considerably depending on the
2.2.1. Salt hydrates surface area of the material to be coated, and other physical
It is defined as the inorganic salts that have water molecules characteristics of the system. Besides, the shell coating material
has to be non-hygroscopic, with medium/low viscosity, and
combined in a definite ratio as part of the crystal, as XnYm aH2O
low cost.
formula, where X is a cation, Y is an anion, and a is the number of
water molecules. They are solid at room temperature, and when
the melting point is reached, the salt starts to dissolve in their own
4. Types of microencapsulated phase change materials (MPCM)
water crystal.
There are several studies about MPCM, where choosing the
2.2.2. Salts combination shell/core is the most important point. The propor-
They are inorganic salts with a formula as XnYm, where X is a
tion of core material in the capsule is usually between 20% and
cation and Y is an anion. These salts are used for higher tem- 95% by mass [46]. The microcapsules may consist on a single
perature ranges but they have lower enthalpy than salt hydrates. particle or clusters of particles.
An example of a high temperature energy storage use is in a Paraffin wax is one of the most employed PCM in MPCM sys-
concentrated solar power (CSP) plant, which uses salt to store tems. Among paraffin, n-octadecane is the PCM most used
energy for later use. microencapsulated in building applications [47–51].
Fig. 3. Possible morphologies of microcapsules (a) irregular shape; (b) simple; (c) multi-wall; (d) multi-core; and (e) matrix particle.
Fig. 4. Scheme of the types of MPCM, adapted from [66] (a) mononuclear; (b) polynuclear; (c) matrix encapsulation; and (d) multi-film.
There are a lot of studies about the shell. One possibility is the b. Polynuclear: many cores coated with a continuous shell
transparent and thermoplastic acrylic polymer for the shell [42, material.
52–55], such as poly(methyl methacrylate) (PMMA) [56–60]. It has c. Matrix encapsulation: in which the core material is distributed
good mechanical properties and good protection against the homogeneously into the shell material.
environment. For these reasons, PMMA is an adaptable material d. Multi-film: a continuous core coated with multilayer con-
and it is a good polymer as shell material in the preparation of tinuous shell material.
MPCM for thermal energy storage applications. Moreover, as
s
example of commercial MPCM, BASF has a variety of products There are three different methodologies to microencapsulate
s
with PMMA as shell material. As examples of studies with BASF PCM based on the mechanisms of microparticle formation: che-
materials, Tzevetkov et al. [61] studied one of the products, mical, physical and chemical, or physical and mechanical mode.
s
Micronal , using scanning transmission X-ray spectromicroscopy.
This PMMA has good compatibility with a wide variety of PCM, for
5.1. Chemical methodology
example with fatty acids, such as stearic acid, palmitic acid, myr-
istic acid and, lauric acid as studied by Alkan et al. [62]. Besides,
Suspension, dispersion, emulsion, in situ and interfacial poly-
Giro-Paloma et al. [63] evaluated in detail the physical, chemical
s merization, or polycondensation are different procedures widely
and mechanical properties of Micronal DS 5001.
employed for the fabrication of PCM microcapsules (MPCM).
Another polymeric shell very employed is the melamine–for-
Table 2 enumerates the advantages and the drawbacks of each
maldehyde (MF). Su et al. [64] studied the influence of the tem-
procedure.
perature in the deformation, concluding that the yield point of
MPCM decreased with the increasing of temperature. Also, Pala-
5.1.1. Suspension polymerization
nikkumaran et al. [65] used the MF shell to contain n-octadecane
Sánchez-Silva et al. [67] exposed that the suspension poly-
as PCM using the in-situ polymerization technique.
merization process is governed by multiple simultaneous
In Table 1a list of some manufacturers0 trademark name, the
mechanisms such as particle coalescence and break-up, secondary
PCM they use, the shell material, and the particle size distribution
nucleation, and the diffusion of monomer to the interface. The
(PSD), and its application is shown.
collective effect of these mechanisms confers the size, the struc-
ture and the surface properties to the microcapsules. Fig. 5 shows
a scheme of the suspension polymerization methodology. Sánchez
5. Methods to encapsulate PCM
et al. [68] developed a method based on a suspension free radical
polymerization process to fabricate microencapsulated non-polar
The system core/shell is a key point in the fabrication of
microcapsules, being the shell function to protect the core, and the PCM. The same authors [69] investigated the influence of the
core function to contain the active material, in this case the PCM. reaction temperature, the stirring rate and the mass ratio of par-
The MPCM0 s morphology can be diverse as Fig. 3 shows, but the affin to styrene on the thermal properties of MPCM. Borreguero
most common are the spherical and the irregular ones. et al. [70] considered the microencapsulation by suspension
The microcapsule description and their morphology depend on polymerization with gypsum in two steps: a continuous one
the core material and the deposition process of the shell. There are formed by deionizated water and the stabilizer (Polyvinyl-pyrro-
four types, as Fig. 4 shows: lidone, PVP), and a discontinuous one containing the styrene
monomer, the paraffin wax and the benzoyl peroxide. As main
a. Mononuclear (core/shell): a single core wrapped with a con- result they achieve an improvement of the thermal insulation
tinuous shell material. capacity of the gypsum by the addition of the prepared MPCM.
5.1.2. Dispersion polymerization process no reactive agents are added to the core material and
Dispersion polymerization is a very attractive method due to its polymerization occurs exclusively in the continuous phase. This
inherent simplicity of the single-step process. Typical examples of method to microencapsulate PCM has to have all the materials for
this method are the dispersion polymerization of styrene in the microcapsule wall originate from continuous phase of the
hydrocarbons, alcohols, alcohol–ether and alcohol–water mix- emulsion system, and have to be water soluble [76]. Initially a low
tures. In this methodology it is important to control the para- molecular weight pre-polymer will be formed, as time goes on the
meters such as initiator, monomer, stabilizer concentration, and pre-polymer grows in size, it deposits on the surface of the dis-
the reaction time on the characteristics of the final particles with persed core material thereby generating solid capsule shell [77].
this methodology. One way to do it is by UV photo-initiated dis- First, a PCM emulsion is prepared and then the synthesis of the
persion polymerization of stearic acid in PMMA shell as described pre-polymer solution is carried out through the mixture of two
by Wang et al. [71], which has high efficiency as they exposed in polymers, which will form the cover, and water. This pre-polymer
their study. Kim et al. [72] show that monodisperse poly(methyl is added to the emulsion in the form of droplets, while the
emulsion is agitated during a specific time. The emulsion is cooled
methacrylate) microspheres were successfully synthesized by the
and filtered, obtaining the microcapsules, which have to be dried.
dispersion polymerization using hydrophilic polyvinylalcohol
To enhance the mechanical properties, it is suggested to add
(PVA) in a methanol/water mixture media. Fig. 6 presents a gra-
modifying agents [78]. Boh et al. [79] have used a modified in situ
phic description of the dispersion before and after the poly-
polymerization method with melamine–formaldehyde pre-
merization process.
polymers as wall materials and styrene–maleic acid anhydride
copolymers as modifying/emulsifying agents. Furthermore, Boh
5.1.3. Emulsion polymerization
et al. [80] define this technique as the procedure where monomers
This method consists of mixing the polymer in an oiled system,
or pre-condensates are added only to the aqueous phase of
adding an emulsifier. After this, an emulsification is needed, to
emulsion. Moreover, Yang et al. [81] studied the best shell to
create a water/oil emulsion and to generate a crosslinked system
encapsulate tetradecane as PCM with polystyrene (PS), PMMA,
(chemically, thermally, or in an enzymatic way). The final step is
poly(ethyl methacrylate) (PEMA) and polyvinyl acetate (PVAc) as
washing the emulsion, to remove the oil and to create the isolated Phase Change Slurries (PCS) using this technique, and the study
microcapsules. In Fig. 7a scheme of this methodology can be concludes that PMMA and PEMA are the best shells. After this
observed. Sarı et al. [74] used this technique to prepare and study, Yang et al. [82] had used the same PCM contained in dif-
characterize the MPCM for TES of PMMA as shell and n-heptade- ferent shell materials, Acrylonitrile–styrene copolymer (AS),
cane as PCM. acrylonitrile–styrene–butadiene copolymer (ABS), polycarbonate
(PC), concluding that all the three shell materials could be used to
5.1.4. In situ polymerization microencapsulate n-tetradecane. Using this same PCM, Fang et al.
In this methodology the capsule shell formation occurs because [83] encapsulated it with urea and formaldehyde, concluding that
of the polymerization of monomers added to the reactor. In this the n-tetradecane encapsulation is efficient with good thermal
stability and attractive for thermal energy storage and heat
Table 2 transfer applications. Besides, Chen et al. [84] synthesize and
Techniques for chemical methodology in microencapsulation process.
characterize MPCMs made of paraffin/SiO2 obtained by this pro-
Technique Advantages Disadvantages cess, being a good MPCM because the SiO2 protect the paraffin
Suspension Good heat control of the Few monomers are water

polymerization reaction soluble. Size around 2 –
Cost effective 4000 μm [107]
Dispersion Micron-size monodisperse Not reported
polymerization polymer particles in a sin-
gle batch process
Emulsion High MW polymer fast Purify polymer from the
polymerization surfactant
In situ polymerization Uniform coating. Size between 1 and
2000 μm
Interfacial Versatile, good properties Size MPCM 2–2000 μm
polymerization in size, degradability,
mechanical resistance
Fig. 6. Schematic description of dispersion polymerization [73].
Continuous phase
Monomers, initiator
stir
heat
Surfactant molecule
Continuous phase with

surfactant
Fig. 5. Scheme of the suspension polymerization microencapsulation process.
Oil + Emulsifier
Crosslinking
Polymer
Water/oil MPCM
emulsion formation
Fig. 7. Scheme of the emulsion polymerization microencapsulation method. Adapted from [75].
Table 3
Encapsulation techniques for physical and chemical methodology.
high P +
Technique Advantages Disadvantages
homogenization
Coacervation Two methods Agglomeration
Versatile
Good control of the particle Difficult to scale-up
monomer B size and thickness
Sol–gel encapsulation Inorganic shell with high Still under research
thermal conductivity
Water/Oil emulsion with MPCM Supercritical CO2- Effective and green method Not very used
assisted Cost effective
monomer A
Fig. 8. Scheme of the Interfacial polymerization microencapsulation method.
Adapted from [89]. where it is highlighted that high pressure is needed to
obtain MPCM.
from reacting with the outside environment. Finally, there is a Table 2 shows the advantages and disadvantages of the differ-
study of Song et al. [85] where MPCM with hexadecane as core ent techniques for chemical methodology described.
material were prepared by this methodology by using urea–for-
maldehyde resin and urea–formaldehyde resin modified with 5.2. Physico-chemical methodology
melamine as shell materials respectively, concluding that the
addition of melamine into the urea–formaldehyde resin reduced It includes coacervation, layer-by-layer assembly, sol–gel
the microcapsule size and the microencapsulation efficiency. encapsulation and supercritical CO2-assisted methods. Table 3 lists
Moreover, the effects of the system concentration, the agitation the advantages and disadvantages of each technique in the
speed and mass ratio of the wall are key factors to take into physico-chemical methodology.
account, as it is referred in the last references.
5.2.1. Coacervation
5.1.5. Interfacial polymerization There are two methods for coacervation process, the simple
In this technique the shell capsule is formed at or on the sur- one and the complex one. The microcapsule formation mechanism
face of the droplet or on the particle by polymerization of the for both processes is the same, with the exception on the way in
reactive monomers, and involves dispersing an organic phase which the phase separation is carried out. For simple coacervation,
(containing poly-functional monomers and/or oligomers) into an a desolvation agent is added for phase separation. By contrast, a
aqueous phase (containing a mixture of emulsifiers and protective complex coacervation involves complexation between two oppo-
colloid stabilizers) along with the material to be encapsulated. The sitely charged polymers. Fig. 9 shows a scheme of this procedure.
presence of crosslinks affects the morphology of the external Besides, there are three steps in complex coacervation. The first
microcapsule surface [86]. The substances used as a shell are step is the formation of three immiscible phases, the liquid man-
multifunctional monomers. The multifunctional monomer is dis- ufacturing vehicle, the core material, and the coating material. The
solved in liquid core material and it will be dispersed in aqueous core material is dispersed in a solution of the coating polymer. It is
phase containing a dispersing agent. Generally, used shell forming needed a changing temperature of polymer solution and a addi-
material includes co-reactant multifunctional reagent like dia- tion of salt, nonsolvent, and of an incompatible polymer to the
mines, isocyanates and diacid chlorides. These results in rapid polymer solution. The second step is the deposition of the coating,
polymerization at the interface and the generation of the capsule and the third step is the coating rigidization. The prepared
shell takes place [77]. The main advantages of this technique are microcapsules are stabilized by crosslinking, desolvation or ther-
the high reaction speed, mild reaction course, and also that its mal treatment. Fig. 10 shows the steps involved in the complex
products have low penetrability. Liang et al. [87,,46] succeed with coacervation technique.
the interfacial polymerization to prepare MPCM of butyl stearate In the complex process, the polymeric solute is separated in the
as a PCM in a polyurea system. Li et al. [88] fabricated nano- form of small liquid droplets, forming the coacervate. Then, it is
particles of SiO2/paraffin using this process of polymerization and deposited around the insoluble particles dispersed into a liquid.
concluded that the methodology can be extended to fabricate These droplets slowly unite and form a continuous cover around
other organic and inorganic PCM with different core/shell com- the core. In order to obtain a longer lifetime of microcapsules, this
positions. Fig. 8 shows a scheme of interfacial polymerization technique can be completed in two steps, adding the polymer
twice. Through this mechanism, a smaller thickness of the compared with urea–formaldehyde resin, melamine–for-
microencapsulate shell can be obtained. Compactability and maldehyde resin, and β-naphtol–formaldehyde.
impermeability are improved (a lower speed of polymer deposi-
tion increases impermeability), giving greater stability to the 5.2.2. Sol–gel encapsulation
microcapsules, conserving size and spherical form. The texture is This methodology is described as the formation of an oxide
smoother and the spherical form is more regular, compared to association through polycondensation reactions of a molecular
one-step coacervation, where microcapsules with many protru- predecessor in a liquid. A sol is a stable dispersion of polymers or
sions, rougher, coarser and more porous are obtained. Hence, it is a colloidal particles in a solvent, where the particles can be crys-
phenomenon which takes place in colloid systems, where mac- talline or amorphous. On the other hand, a gel consists on a three
romolecular colloid rich coacervate droplets surround dispersed dimensional continuous network, which includes a liquid phase,
microcapsule cores, and form a viscous microcapsule wall, which building an agglomeration of colloidal particles. Besides, in a
is solidified with cross-linking agents. Özonur et al. [91] used this polymer gel the particles have a polymeric substructure composed
technique concluding that gelatin þArabic gum mixture was the by aggregates of subcolloidal particles. In general, the sol particles
best wall material for microencapsulating coco fatty acid mixtures interact by Van der Waals forces or hydrogen bonds, but can also
be formed from linking polymer chains. Fang et al. [92] used the
sol–gel methodology to prepare form stable lauric acid/silicon
dioxide composite PCM. This material can be used for TES in waste
heat recovery as well as solar heating systems. Li et al. [93], using
the sol–gel methodology, prepared a shape-stabilized paraffin/
silicon dioxide composite PCM. Also, Tang et al. [94] enhanced the
thermal conductivity of PEG/SiO2 via in situ chemical reduction of
CuSO4 through ultrasound-assisted sol–gel process, concluding
that the Cu/PEG/SiO2 hybrid material have excellent thermal sta-
bility and a good-stable performance. Fig. 11 shows a scheme of
the sol–gel process.
5.2.3. Supercritical CO2-assisted

Supercritical carbon dioxide has attracted a great deal of
attention as an alternative to the conventional processing because
it is an effective and green synthetic method. Supercritical CO2-
assisted have gained a strong interest in the synthesis of polymeric
composites because it has low critical temperature value, is non-
toxic and has non-flammable properties. Moreover, it is readily
available, highly pure and cost-effective. Wu et al. [96] used this
technique studying the effects of some factors on the particle size
of PMMA particles prepared via a supercritical assisted-
atomization (SAA) process using acetone as a solvent and super-
critical carbon dioxide as a spraying medium. These factors
included the concentration of polymer solution, temperature in
saturator and volumetric flow rate ratio of carbon dioxide to
polymer solution. More recently, Haldorai et al. [97] has sum-
Fig. 9. Scheme of simple coacervation technique, where (a) the core material is
dispersed in a shell polymer solution; (b) the separation of the coacervate from the
marized on the synthesis of polymer-inorganic filler nanocompo-
solution; (c) coating of core material by coacervate droplets; and (d) coalescence of sites in supercritical CO2 and conclude that although there are
coacervate to form continuous shell around core particles. Adapted from [90]. three methods for the preparation of nanocomposites (blending,
Oil
Gelatine solution
50 ºC Crosslinking
Washing
Cool down slowly
Encapsulant
Adjust pH
Dispersing +
mixing
Fig. 10. General processing scheme for microcapsule preparation by complex coacervation using gelatin and Arabic gum.
Solution of Sol Gel

precursors
Fig. 11. Sol–gel process microencapsulation method, where (a) is the condensation, and (b) is the gelation. Adapted from [95].
Table 4 5.3.3. One-step method

Scheme for physical and mechanical methodology in microencapsulation process. The benefits of using this method include easy scale-up and no
need for a stabilizing agent due to self-stabilization. It allows
Technique Advantages Disadvantages
tuning of the size and polydispersity of the capsules, and the use of
Spray-drying Easy to scale-up High temperature different core materials. Jin et al. [102] uses this methodology
Versatile Agglomeration of particles without surfactants or dispersants nor acids/bases for stabilizing
Low cost Remaining uncoated the capsules via oil/water emulsion, and the obtained results
particles
shows that the method allows tuning of the size and poly-
Electrostatic Spherical Only for o50 μm
encapsulation microbeads dispersity of the capsules, and the use of different core materials.
One-step method Easy to scale-up –
Self-stabilization –
6. Phase Change Slurries
sol–gel and in situ polymerization), the super-critical CO2 has been
Phase Change Slurries (PCS) [103] is another important part of
demonstrated to be a viable alternative to the conventional
MPCM [104,105]. When the MPCM is fabricated in a dried state
solvents. [106,107] it can be mixed with a carrier fluid, mainly water [108]
or with other substances such as glycol [109,110] or glycerol
[111,112], creating a PCS. These are widely employed in several
5.3. Physico-mechanical methodology
fields, such as pumping active systems [113,114], using them for
refrigeration [103,115], in air conditioning [116,117], in heat
It include spray-drying, electrostatic encapsulation, and one-
exchangers [118], heating [119], ventilation and air-conditioning
step method. These techniques are inherently not capable of
(HVAC) [116,120,121], in solar energy [122], in cold storage [123],
producing microcapsules smaller than 100 μm [66]. In Table 4 the
and heat exchangers [118] applications. As Salunkhe et al. review
benefits and disadvantages of each technique in the physical and [124], the PCS not only acts as an energy storage device but also as
mechanical methodology is listed. a heat transport system. The way of pumping the slurries in an
active system is very important [113,125], because it is know that
5.3.1. Spray-drying microcapsules can broke when they collide ones to each other.
it is a low-cost commercial process which consists on the Moreover, Zeng et al. [126] studied numerically the influences of
preparation of an emulsion, dispersing the material of the PCM in microparticles and phase change in fluid-pure water, PCS and
a concentrated solution of the material forming the capsule, until MPCM. Besides, Huang et al. [127] and Günter et al. [128] studied
the desired size of the microcapsule is achieved. Then, this the subcooling in PCM emulsion, remarking that in PCS applica-
emulsion is pulverized into droplets. Afterwards, it will be dried, tions, the changed nucleation and solidification behavior is critical.
evaporating the water, which let the active material to be trapped
inside a film of encapsulating material. This technique involves the
atomization of a homogeneous liquid stream in a drying chamber 7. Characterization of MPCM
where the solvent is evaporated and solid particles are obtained. It
is suitable for heat-sensitive materials. This technique was studied 7.1. Experimental characterization techniques reported in the study
of MPCM
by Borreguero et al. [98] mixing LDPE and EVA to create the
polymeric shell. They chose these two polymers due to their
7.1.1. Particle size distribution (PSD)
similarity of the chemical structure, besides the low density, their
For the evaluation of the microspheres0 size and the percentage
versatility, and the inexpensive cost. Moreover, Hawlader et al.
in number or in volume of each size, is used laser diffraction
[99] and Fei et al. [100] used also this technique to produce other spectrometry. The results must be evaluated taking into account
types of microcapsules, using different shells (formaldehyde and the size as well as the transparency of the MPCM, so there are two
titania, respectively), and cores (Gum Arabic, paraffin wax, and mathematical models to do so: Mie and Fraunhofer [129]. Mie
n-octadecane, respectively). model fits better for homogenous and spherical particles, opaque
or transparent and with diameters below 30 μm. Also, to calculate
5.3.2. Electrostatic encapsulation the size of the microcapsule it is needed the refractive index and
This technique is effective for production of particles, around the absorption of the substance. For using the Fraunhofer model is
100 μm. It might be used to prepare spherical microbeads with a needed opaque particles bigger than 30 μm. Most of the MPCM
hydrophobic core and a hydrophilic or hydrophobic shell [101]. evaluation studies included this technique. Yu et al. [130] used this
Table 5
Thermal properties.
Ref MPCM PCM content (%) Latent heat [J g 1] Phase change (°C) peak temperature Diameter (μm)
[5] PS þ paraffin wax – 104.7 40 45 5.5

[48] PMMA þn-octadecane – 198.5 197.1 29.2 33.6 0.05–0.3
PEMA þ n-octadecane – 208.7 205.9 31.1 32.3 0.06–0.36
[52] PMMA þdocosane – 54.6 48.7 41 40.6 0.16
[54] Acrylate/butyl stearateþ paraffin 48–68 85 – 10–30
[57] PMMA þeicosane 35.2 34.9 54.2 87.5 0.7
[58] PMMA þn-hexadecane 29.04-61.4 68.89 and 145.61 – 0.22–1.050
[59] PMMA þparaffin 106.9 112.3 55.8 50.1 0.21
[60] MMA þ n-pentadecane – 107 97 10 9.5 650–760
[62] PMMA þSA 80 187 190 67 66 –
PMMA þPA 80 173 175 60 59 –
PMMA þMA 80 166 168 51 50.7 –
PMMA þLA 80 149 151 41 41.5 –
[67] Melamine–formaldehyde þparaffin – 87.5 45 380
[81] PMMA þPCM – 66.26 60.62 2.95 5.97 5–30
PEMA þ PCM – 80.62 65.35 3.19 5.68 6–30
[82] Acrylonitrile–styrene copolymerþ n-tetradecane – 142.3 10 o1
ABSþ n-tetradecane – 107.1 10 o1
PC þn-tetradecane – 49.5 10 o1
[83] Urea/formaldehyde þ n-tetradecane 60 134.16 – 0.1
[84] SiO2 þ paraffin – 156.86 144.09 57.96 55.78 40–60
[87] Polyurea þbutyl stearate – 80 29 20–35
[88] paraffin þSiO2 – 45.5 43.8 56.5 45.5 0.2–0.5
[92] SiO2 þ polyethylene glycol – 117.21 90 44.78 40.33 –
[93] SiO2 þ paraffin – 35.8 32.51 57.8 56.85 –
[102] Silica þ nonadecane- – 124.7 – 27
[100] LDPE/EVA þRT27 49.32 98.14 25.42 31.15 3.5
Polystyreneþ RT27 48.61 96.14 26.12 30.28 360
[122] BASF slurries – – up to 70 ºC 2–8
[127] RT-20 emulsion 21.2 – 0.2-12.5 –
[130] MFþ n-dodecanol – 187.5 21.5 30.6
[131] Gelatine/Arabic Gum þRT-27 – – – 9
Sterilized Gelatine/Arabic Gumþ RT-27 – 79 25.15 28.15 12
Agar-Agar/Arabic Gum þ RT-27 – 78 26.35 29.35 4.3
[135] Polystyreneþ n-octadecane – 124.4 – 0.100–0.123
[136] MFþ n-octadecane – 122.5 132.2 26.75 20.33 12.45
[138] Polycarbonateþ Stearic acid – 91.4 96.8 60.2 51.2 0.5
[167] HDPE þ paraffin 96.79 37 55 300
[173] Polysiloxane þn-eicosane – 139 37.4 30 22.9
[186] Micronal (BASF) 100 26 5
technique to study the diameter distribution of MPCM prepared 7.1.5. X-Ray diffraction (XRD)
with different mass ratios of emulsifier to PCM. This technique is used to analyze the crystalloid phase of the
microencapsulated paraffin, like Fang et al. [134] show in their
7.1.2. Optical microscopy (OM) study, synthesizing and characterizing MPCM paraffin composites
This technique provides images of microspheres with a good with SiO2 shell. Moreover, this technique is used to assure the
resolution, allowing the evaluation of their morphology, fixation, encapsulation of the PCM, as Fang et al. [135] used XRD patterns of
durability, and without a complex sample preparation. Sánchez n-octadecane, styrene and the nanoencapsulated PCM, suggesting
et al. [5] used in their study transmitted light and reflection mode that n-octadecane was successfully encapsulated by the shell of
to develop thermo-regulating textiles using MPCM of paraffin in polystyrene. So, this technique plays an important role on studying
the core. Besides, Bayés-García et al. [131] characterize MPCM with the prevention of leakage of PCM.
Gelatine/Arabic Gum (G/AG) by using a thermo-optical microscope
7.1.6. Wide angle X-ray scattering (WAXS) and low angle laser light
at different temperatures.
scattering (LLALS)
The crystalline structure of polymers and PCM can be examined
7.1.3. Scanning electron microscopy (SEM)
by this technique. It is convenient to evaluate the crystallographic
This technique is essential to evaluate the shape and size of the
forms of the encapsulated PCM. Zhang et al. [136] analyzed the
MPCM. Besides it is useful to study the surface of the micro-
WAXS patterns of the MPCM with different weight ratios of core/
capsules, as well as if there is PCM spread. It is a fast technique and
shell (n-octadecane/resorcinol-modified melamine–formaldehyde)
it is widely employed. Bajare et al. [132] studied the shell thickness materials. Moreover, Sánchez-Silva et al. [67] had used LLALS tech-
s s
of BASF Micronal DS 5001 by using this technique. nique to better characterize the MPCM styrene–methyl methacrylate
copolymer shell.
7.1.4. Transmission electron microscopy (TEM)
The morphology and the structure of the microcapsules can be 7.1.7. Fourier transformed infrared spectroscopy (FT-IR)
observed also by TEM, when their size is below micrometers, as This technique is used to evaluate the microcapsule shell
Pan et al. [133] evaluated for nanostructures prepared through in- material, as well as to study the possible degradation of the
situ interfacial polycondensation, resulting colloidal sphere external part of the microsphere. It can be analyzed by Attenuated
microcapsules with diameter around 200 nm. Total Reflectance (ATR) or with a KBr pellets [137]. An example of
this use is the study of Zhang et al. [138] whom characterize the (using mathematical models) to predict the quality of indoor air.
polycarbonate shell before and after 1000 thermal cycles to eval- There are some others studies about the outdoor environment
uate the matrix thermal distortion temperature. [155,156]. Also, it is studied that multi-layer materials have much
longer VOC0 s emission time and a slower VOC0 s decay rate com-
7.1.8. Differential scanning calorimeter (DSC) pared with single-layer materials [157]. Moreover, it has to take
This is one of the most popular thermal analysis techniques. It into account that the adsorption/desorption phenomena of rela-
measures endothermic and exothermic transitions in function of tively high vapor pressure compounds are negligible in building
the temperature. It also can detect glass transitions, fusion, crys- [158]. Besides, the percentage of approximately 40% of the indoor
tallization, and oxidation. It can measure specific heat capacities
air quality levels originated from building materials [159] are
[139]. For these reasons, this technique is widely employed to
VOC0 s associated with the perception of bad odors. In buildings
characterize the thermophysical properties of MPCM. It provides
which are renovated or new (considering new buildings that are
the melting and solidifying temperature, as well as, the melting
less than 10 years old) the levels of indoor air pollutants are higher
and solidifying enthalpy of a sample, revealing if the material has a
than the VOC0 s levels in aged buildings [160].
good capacity to store energy. Ostrý et al. [140] confirmed by DSC
Implementing MPCM in gypsum board, concrete, plaster or
technique the suitability of some PCM for their integration in
building structures. Table 5 summarizes the main thermal prop- other wallboard material, thermal storage can be a part of con-
erties (latent heat and phase change peak temperature) of the struction technology for light weight buildings, and the MPCM
MPCM analyzed in this review, describing the composition of the could be used for high density thermal energy storage [161,162],
core and shell material. so the final product would achieve energy savings in buildings.
The fact of using gypsum, cement and heavyweight sheet with
7.1.9. Thermogravimetrical analysis (TGA) PCM could produce some VOC0 s in the indoor air in a cubicle
This technique measures the amount and rate of change in the [163,164]. Consequently, it is important to preserve the air quality
weight of a material as a function of temperature or time in a of a room. Hence, it is used MPCM to reduce the toxic effects that
controlled atmosphere. Measurements are used primarily to could be expelled in a system [165]. Although using MPCM mixed
determine the composition of materials and to predict their with other constructive materials, there is a main concern on the
thermal stability. The technique characterize materials that exhibit use of organic PCM because of the possible emission of volatile
weight loss or gain due to decomposition, oxidation or dehydra- compounds [156,166]. Due to most commercial PCM micro-
tion and also their thermal stability. There are a lot of studies using capsules have not been well characterized for volatile emission, a
it. Zhang et al. [141] evaluate the step thermal degradation of a proposition for future studies could be to characterize and mea-
silica/n-octadecane MPCM, as well as the thermal reliability by sure the volatile organic compounds for PCM, MPCM and con-
using this technique. structive materials containing these kind of materials.”
7.1.10. Atomic force microscopy (AFM)

It is a surface technique which has the ability to obtain topo- 7.2. Properties to analyze
graphic images of surfaces with nanometric resolution. It can be
used as a nanomanipulator in order to move and test the surface of 7.2.1. Flammability
the samples in a variety of ways, such as electrically, magnetically Due to the lower thermal stability and inflammability proper-
and mechanically. The microcapsules0 mechanical properties can ties of MPCM, their usage has been severely restricted especially in
be evaluated by using this technique. The microcapsule maximum building applications [50]. For this reason, the studies of deter-
force and the total deformation of an individual microcapsule [98] mining the flammability properties of MPCM are of importance in
have to be measured increasing the applied force until obtaining many applications. The Cone calorimeter is one of the most
the typical force displacement curves. It is necessary to repeat this effective bench scale methods for investigating the combustion
procedure several times (at least 3 times). Furthermore, it can be properties of polymer materials. Cai et al. [167] evaluate this
extracted the deformation histogram and Young0 s modulus histo- property on form-stable PCM based on paraffin/high density
gram taking into account a small area on the top of the micro- polyethylene (HDPE) composites with expanded graphite (EG) and
capsule. Giro-Paloma et al. [142] evaluated the maximum force ammonium polyphosphate (APP) flame retardant system.
that a dried PCS can support on the top of the microsphere using
atomic force microscopy (AFM) technique. Besides, Giro-Paloma 7.2.2. Viscosity measurement, density, and conductivity
et al. [63] also evaluated the maximum force that the MPCM The viscosity of melted PCM or PCS is very important in flow-
s
Micronal DS 5001 can support before their breakage at three
age and is important to measure it at different temperatures with
different temperatures: 25 °C, 45 °C and 80 °C by using this tech-
a rotation viscosimeter. High viscosity will increase the pump
nique. They conclude that the required applied load in order to
energy consumption.
break the sample depends on the working temperature. Hence, the
Another important property to take into account in a PCS sys-
temperature is a key point to take into account when a PCM have
tem is the density (ρPCS) which is given by Eq. (1), where Xi is the
to be chosen for a specific application.
weight fraction and ρi is the density of each component:
7.1.11. Emission of volatile organic compounds 1
The volatile organic compounds (VOC0 s) evaluation at different ρPCS ¼ P xi ð1Þ
ρi
temperatures is an important issue to better characterizing PCM i
and MPCM. Materials for indoor environments should not emit
hazardous gases in the form of volatile organic compounds. There Density can be obtained by using a specific gravitymetre or a
are studies over the past decade of measuring the air quality pycnometer by determining the volume.
(indoor environment) in building materials through volatile Another property used to characterize MPCM and PCS is the
organic compounds (VOC0 s) because they play a major role in thermal conductivity (k), which can be calculated in different ways,
construction [143–154]. Therefore, the VOC0 s emission from as Youssef et al. [94] report in their review. One way to calculate the
building materials can be studied experimentally and theoretically thermal conductivity of a MPCM is by Maxwell0 s et al. [168]
relation: results obtained from gypsum based composite material containing

BASF MPCM.
2 þ KKMPCM þ 2CMPCM KKcont
MPCM
1 Cabeza et al. [161] and Castellón et al. [185] developed a new

cont
K MPCM ¼ Kcont ð2Þ
2 þ KKMPCM CMPCM KMPCM innovative concrete with microencapsulated phase change mate-
cont Kcont 1
rials (MPCM) without losing any of the initial concrete character-
Furthermore, Wang et al. [169] evaluated these three properties istics and achieving high energy savings in cooling. The experi-
in a microencapsulated phase change material (MPCM) slurry flow mental setup used consisted of two identically shaped cubicles of
in a circular horizontal tube. The viscosity was evaluated as well as concrete, one with conventional concrete, and the other one with
the density of the slurry, which was calculated by weighted frac- the modified concrete which included MPCM. The MPCM used was
s
tion of the densities of PCM, the coating material, and the water, a commercial microencapsulated PCM called Micronal PCM (from
based on the mass and energy balance. The thermal conductivity BASF) with a melting point of 26 °C, and a phase change enthalpy
of the microcapsule was calculated based on a composite sphere of 110 kJ kg 1. The developed concrete reached a compressive
approach. strength over 25 MPa and a tensile splitting strength over 6 MPa
(after 28 days). Moreover, concrete panels were produced in a way
7.2.3. Cycling close to common concrete production methods. The results of this
The thermal cycling test reveals the thermal reliability and study showed improved thermal inertia as well as lower inner
chemical stability of a microcapsule [170]. For this reason, it is an temperatures, demonstrating a real opportunity in energy savings
essential test to evaluate the quality of the microcapsules to assure for buildings.
the no alteration on its geometrical profile after several cycles One of the main drawbacks found in this experimentation was
[171,172]. The thermal reliability can be evaluated in a DSC device, the severe influence of high outdoor temperature peaks and solar
as Fortuniak et al. [173] used to withstand 50 fusion-crystallization radiation over the PCM during the summer, which prevented its
cycles tests, or in a thermocyclator. There is another study by Sarı solidification during night and thus diminished its achievable
et al. [56] where it was tested the thermal cycling test with 5000 potential benefits. Therefore, Arce et al. [9] tried to overcome such
cycles of a PMMA shell and n-octacosane PCM. a problem and to increase the operation time of the PCM and the
thermal comfort achieved. For such a purpose, in 2008–2009
similar experiments have been performed with awnings added to
the set-up, providing them with solar protection. Results showed
8. MPCM applications
that peak temperatures were reduced about 6%. Moreover, PCM
remained active for at least 4% more hours, and the comfort time
In between the applications of MPCM, the use of MPCS for
was increased at least 10% in cubicles with awnings.
cooling in Narita Airport (Tokyo, Japan) can be found [115]. Here
MPCM was also added to sandwich panels [186] to increase their
MPCS was used to compensate the decrease of energy capacity
thermal inertia and to reduce the energy demand of the final
caused when the refrigerant was substituted due to environmental
buildings [184]. To manufacture the sandwich panel with micro-
reasons. The slurry used is the mixture of water and 2 μm micro-
encapsulated PCM three different methods was tested. In case 1, the
capsules, and the melting temperature and the corresponding
PCM was added mixing the microencapsulated PCM with one of the
latent heat of which are 8 °C and 75.9 kJ kg 1, respectively. The
components of the polyurethane. In the other two cases, the PCM
storage tank is 24.7 m in height and 7.4 m in diameter. Cold energy was added either a step before (case 2) or a step after (case 3) to the
is stored during night time and released during day time. addition of the polyurethane to the metal sheets. The results show
Another interesting application of MPCM is in buildings. Here that in case 1 the effect of PCM was overlapped by a possible
active and passive systems can be considered. In active systems, increase in thermal conductivity, but an increase of thermal inertia
MPCS are involved, since the MPCM needs to be movable. Griffiths was found in case 3. In case 2, different results were obtained due to
et al. [174] investigated the use of MPCS in a ceiling panel. MPCS the poor distribution of the PCM. Some samples showed the effect
with a melting temperature of 18 °C and 2–8 μm microcapsules of the PCM (higher thermal inertia), and other samples results were
produced by BASF (40% concentration) was used as heat transfer similar to the conventional sandwich panel. In both cases (2 and 3),
medium in a test chamber (with working temperature of 16–18 °C). it is required to industrialize the process to improve the results. In
As for passive systems, MPCM have been combined with dif- these experiments, 8% in weight of MPCM with respect to the
ferent building materials, such as gypsum, concrete [139,165,175– s
weight of the PUR was added. Here also Micronal PCM (from BASF)
179], and insulating materials, and tested in different set-ups. In with a melting point of 26 °C was used.
2005, Schossig et al. [180] presented the results of adding PCM in Similarly, Borreguero et al. developed new rigid polyurethane
plaster and testing the new product in real offices. Since com- foam containing microencapsulated Rubitherm RT27 [187]. 21 wt%
parison was quite difficult due to the influence of users, two new content of MPCM could be incorporated in RPU foams, improving
full-size test rooms with a lightweight construction at the facade the TES capacity of these materials but depressing their mechan-
testing facility and coated the interior walls with PCM plaster and ical properties. Results indicated that the foaming process was
reference plaster were built. The measured data showed the affected by the microcapsules content decreasing the foam rising
potential for PCM products to reduce the cooling demand and rate and its final size. Later on, they used catalyst Tegoamin 33 in
increase the comfort in lightweight buildings. Later, MPCM the process, being able to include 18 wt% MPCM in the foam
incorporated in gypsum boards has been investigated by many maintaining the mechanical properties of the neat foam, and
researchers [70,181–183]. catalyst Tegoamin BDE, being to include 21 wt% MPCM with higher
The performance of PCM in building structures is usually mechanical resistance than the previous foams [188]. Finally, rigid
investigated via a dynamic building performance simulation. In polyurethane (RPU) foams were synthesized incorporating up to
order to avoid the need of measuring the thermal properties each 18 wt % of two different kinds of thermo-regulating microcapsules
time the composition changes, Toppi et al. derived experimental having a different shell material consisting of polystyrene or poly
s
correlations to calculate the composite material properties as (methyl methacrylate), named as mSP-(PS-RT27) and Micronal
function of its composition [184]. Such correlations may also be DS 5001 , respectively [189]. The type of microcapsules and their
used, when choosing the material composition, in order to obtain content affected the final foam height, which decreased with the
the required properties. The correlations are based on experimental content and particle size. However, the foam rising curve shape
was not dependent on the microcapsules type or content and was Characterization of MPCM has attracted a lot of attention
successfully predicted by means of a model of reaction curve of between researchers and a lot of methods have been used
four tanks in series. Thermal energy storage (TES) capacity of PU depending on the aim of the analysis and the application con-
foams was improved by incorporating both, mSP-(PS-RT27) or sidered. This review describes shortly the main techniques used
s
Micronal DS 5001 , with the values close to those reported in for MPCM characterization at lab scale, including particle size
the literature (16 J g 1) for the highest content. Nevertheless, the distribution, optical microscopy, SEM, TEM, X-Ray diffraction, wide
highest particle size of the microcapsules from PS and the angle X-ray scattering and low angle laser light scattering, FT-IR,
agglomeration of the microcapsules from poly(methyl methacry- DSC, TGA, and AFM, and some properties analyzed such as
late), promoted by their additive SiO2, led to the strut rupture, flammability, viscosity, density and conductivity measurement,
damaging the final mechanical properties. and cycling.
One of the first applications where MPCM was used is in tex- Finally, some applications of MPCM are shortly described.
tiles to enhance thermal comfort in clothes [5,190–193] and, more These are cooling systems, active and passive systems in buildings,
recently, footwear [194]. In this last application, for example, a
and textiles and footware.
nonwoven fabric, three foams and leather, commonly used as
fabrics for shoe manufacturing, were doped with microcapsules
containing phase change materials (PCMs) and also with carbon Acknowledgments
nanofibers (CNFs) in order to improve the thermal comfort pro-
vided by the shoes. The maximum microcapsule content that can
The work is partially funded by the Spanish government
be incorporated and the influence on the weight, thickness and
(ENE2011-28269-C03-02 and ENE2011-22722). The authors would
the thermal properties and behavior of the fabrics were evaluated.
like to thank the Catalan Government for the quality accreditation
The resulting materials showed a thermal energy storage (TES)
given to their research group GREA (2014 SGR 123) and research
capacity up to 13.74 J g 1 and a maximum thickness increase of
group DIOPMA (2014 SGR 1543). The research leading to these
the composite fabric of 0.6 mm. The PCMs addition promoted a
results has received funding from the European Union's Seventh
slight modification of the steady-state temperatures of the fabrics
subjected to heating or cooling processes and the stored and Framework Programme (FP7/2007–2013) under Grant agreement
released heats confirmed that PCMs work in a reversible way. On no. PIRSES-GA-2013-610692 (INNOSTORAGE).
the other hand, the addition of CNFs compensated for the insu-
lating effect of the PCMs. Finally, it was found that footwear con-
taining these materials could hold the foot temperature for a References
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Renewable and Sustainable Energy Reviews 53 (2016) 1059–1075

Contents lists available at ScienceDirect

Renewable and Sustainable Energy Reviews

Types, methods, techniques, and applications for microencapsulated

5.3.1. Spray-drying . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1067

1. Introduction comfort can be used, which is around 20 7̄ C. One of these appli-

ments for the last 10 years (January 2005–April 2015).

These 449 documents related to MPCM were published in 50

Other (7.1 %) Book chapter (0.2 %)

Physics and Astronomy (15.1 %)

Chemical Engineering (23.8 %) Materials Science (30.1 %)

Trademark name PCM Shell material PSD Application

Cristopia Eutectic salts Polyoleﬁn 77 mm Industrial refrigeration, building, conditioning

Suspension Good heat control of the Few monomers are water

Continuous phase with

5.2.3. Supercritical CO2-assisted

Solution of Sol Gel

Table 4 5.3.3. One-step method

[5] PS þ parafﬁn wax – 104.7 40 45 5.5

7.1.10. Atomic force microscopy (AFM)

relation: results obtained from gypsum based composite material containing

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