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Thermochimica Acta 587 (2014) 5258

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Thermochimica Acta

journa l homepage: www.elsevier .com/ locate / tca

Preparation, characterization and thermal properties ofbinary nitratesalts/expanded graphite as composite phase change material

Junbing Xiao a,Jin Huang a,, Panpan Zhu a, Changhong Wang a, Xinxi Lia,b

a School of Materials andEnergy, GuangdongUniversity of Technology, 510006Guangzhou, PR Chinab Center for Nanochemistry, Beijing National Laboratory forMolecular Sciences,State Key Laboratory for Structural Chemistry of Unstable andStable

Species, College of Chemistryand Molecular Engineering, Peking University, Beijing, PR China

a r t i c l e i n f o

Article history:

Received 1 March 2014Received in revised form 18 April 2014Accepted 22 April 2014Available online 29 April 2014

Keywords:

Binary nitrate saltExpanded graphiteUltrasonicThermal energy storageLatent heat

a b s t r a c t

The binary nitrate salts/expanded graphite (EG) composite phase change material (PCM) were preparedvia adding different mass rate ofEG to binary nitrate salts consisting ofNaNO3and KNO3(6:4) by aqueoussolution method adopting ultrasonic. The morphology and chemical composition ofEG and the compos-ite PCM were characterized and investigated by X-ray diffraction (XRD), scan electron microscope (SEM),energy dispersive spectrometer (EDS), transmission electron microscope (TEM), respectively. Laser ther-mal conductivity instrument and differential scanning calorimeter (DSC) were employed to measurethermo physical properties. Drawing the conclusion from investigation, that EG had enhanced thermalconductivity coefficient which largely increased to 4.884 W/(m K) and reduced total latent heat by mostly11.0%. The morphology and phase structure results indicated that EG were well dispersed into and phys-ically combined with molten salts. In general, the prepared composite PCM could be a suitable phasechange material for thermal energy storage.

2014 Elsevier B.V. All rights reserved.

1. Introduction

Since serious shortage of energy resource and tremendousrequirement for renewable energy, phase change material (PCM)with advantageous thermal properties has been applied to satisfythe increasing demand [15]. Depending on the characteristics ofhigh latent heat, high specific heat and high thermal conductivityandso on [6,7], PCM has played an important role in various fieldsextensively [810].

In recent decades, several inorganic PCM and their mixtureshave been investigated for thermal energy storage [1113]. Dueto its better thermal properties, molten salts were usually used asdirect heattransfermedium in industrialapplications[1416]. Var-ious nitrate salts and their composite have attracted tremendous

researchers concern. The mixtures consisting of KNO3, LiNO3andCa(NO3)2 with excellent thermal properties were proved to be apromising PCM [17]. Iverson et al. [18] concluded that temperaturedid not have a significant effect on mechanical properties through

Corresponding author at: B58 100 WestWaihuan Road,GuangzhouHigher Edu-cationMega Center, 510006 Guangzhou, PR China.Tel.: +86 020 39322715;fax: +86 020 39322715.

E-mail address: [email protected] (J. Huang).

analyzing the thermal and mechanical properties of several nitratesalts in common use.

Recently, researches have focused on improving the thermophysical properties of heat transfer and energy storage medium.The usage of different additives is a usual method to obtain bet-ter heat efficiency of molten salts. A kind of inorganic compoundwith the chlorides has given a rise to the thermal conductivitiesof multi-component molten salts composed of potassium nitrate,sodium nitrite and sodium nitrate [19].

According to the excellent thermal and mechanical proper-ties, graphite and EG have been particularly chosen for improvingthermal conductivity of conventional PCM. Rao et al. [20] hadprepared paraffin/graphite composite phase change materials anddemonstrated that the total latent heat value decreased as theincreasing mass rate of graphite. EG/paraffin nanocompositeswere obtained by dispersing EG into paraffin via intensive ultra-sonic irradiation without dispersants. Owing to the distinctivethermal properties of EG, the thermal conductivity of compos-ite increased to 1.04 times higher than that of pure paraffin[21]. Kim et al. [22] had prepared the paraffin/xGnP compositePCM by stirring xGnP in liquid paraffin. An almost linear rela-tionship was concluded between thermal conductivity and massfraction of xGnP. Meanwhile, EG have gained spread applicationin paraffin [23,24] and other organics [25,26] for energy storagesystems.

http://dx.doi.org/10.1016/j.tca.2014.04.0210040-6031/ 2014 Elsevier B.V. All rights reserved.
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J. Xiao et al. / Thermochimica Acta 587 (2014) 5258 53

As EG has benefited the organic on thermal properties, greatefforts have been spent on the mixture of EG and inorganic. Martinet al. [27] had prepared the binary salt consisting of 70wt.% NaNO3and 30wt.% KNO3 and demonstrated that the melting temper-ature ranged from 223 C to 262 C and the enthalpy was about1182 kJ/kg. At room temperature, the apparent conductivitiesof KNO3/NaNO3-graphite made by cold-compression were up to20W/(mK), which was 20 times higher than that of binary salts[28,29]. Xiaoetal. [30] hadreportedthatthe usage of EGto nitrateshad a improvement on thermal conductivity by about 3040% anda reduction on latent heat per mass mixture by nearly 518%.

In present paper, we report a simple and convenient method toprepare the nitrate salts/EG composite PCM by solution methodwith ultrasonic, different from the conventional preparationmethod. The binary nitrate salts were prepared by statically heat-ing NaNO3and KNO3at mass ratio of 6:4 to completely melt. Theultrasonic had played a role of breaking EG into nanoscale slicesand dispersing them into nitrates. The physical combined compos-ite PCM was proved to have excellent latent heat and high thermalconductivity.

2. Experimental

2.1. Materials

Potassium nitrate and sodium nitrate were obtained from sam-ples with A.R. grade and no further purification. Deionized waterand graphite intercalation compounds[31] were self-restraint.

2.2. Preparation

After being dried at 100 C, graphite intercalation compoundswere expanded through a rapid heating in microwave ovens asreported in our previous work [31]. The expanded graphite wasprepared while the bright flame was out.

Potassium nitrate and sodium nitrate were put into an air oven

anddriedat120

C for 24h respectively and thenmixed atthe massratio of 6:4 uniformly. A mixture of binary nitrates salts was placedinto a crucible and then heated at 350C for 30 min statically inorder to melt completely. Afterwards, the crucible was graduallycooleddownto room temperature.The moltensaltswereobtained.Grinding the molten salts slowly and dissolved it in a breaker bydeionized water gradually. Then, EG was added into the previoussolution slowly under continuous stirring at different mass rate.After the EG soaking into the solution, the solution was stirred bythe strong ultrasonichomogeneous instrument(SCIENTZ-IID) witha power of 800W for 1.0h. Then, the breaker was put into a dryingoven and dried at 100 C for 24h. By grinding the dried compos-ite PCM, sample was obtained. Before drying of the solutions, onewas filtered and washed using deionized water until the stripped

graphite flakes (SGFs) were enough visible. SGFs were obtainedafter drying as mentioned.

2.3. Characterization and determination of thermal properties

X-ray diffraction (XRD; DMAX-Ultima IV, Rigaku Corporation,Japan) was employed to identify the microstructure and chemicalcomposition of EG, SFGs and the composite PCM. The morphol-ogyand chemical composition of compositePCM wereinvestigatedby scan electron microscope (SEM; S3400N, Hitachi, Japan) withan energy dispersive X-ray spectroscopy detector, field emissionscanning electron microscopy (FE-SEM; S-4800, Hitachi, Japan)(EDS; EX-250, HORIBA, Japan) at room temperature. The morphol-ogy of SGFs was investigated with a high resolution transmission

electron microscope (HRTEM; JEM-2010HR, Jeol, Japan). Thermal

conductivity of binary nitrate saltsand binary nitrate salts/EG com-posite PCM was measured by employing a laser heat conductiveinstrument (Germany, NETZSCH, LFA 447) at room temperature.The phase change temperature and latent heat of the nitrates andnitrates/EG composite PCM were both measured by differentialscanning calorimetry (DSC; DSC-204, NETZSCH, Germany) undera nitrogen atmosphere. The data were collected with a scan rate of10 Cmin1 from room temperature to 260C.

3. Results and discussion

3.1. Stripped graphite flakes

The morphologies of EG and SGFs were observed by SEM asshown in Fig. 1. As can be seen from Fig. 1a, EG has a 3D worm-like architecture within size of 150m. The high-magnificationSEM photograph (Fig. 1b) of SGFs shows that EG altered to slicesin nanoscale after the ultrasonic.

The TEMphotographsof SGFs from differentangles were shownin Fig. 2. As represented in Fig. 2a, SGFs were flat and semitrans-parent slices with some wrinkles and folds. It could be observedthat its dimension was between 8 and 25nm which corresponded

to observation of SEM photograph in Fig. 1b. As observed in Fig. 2b,the folds with lamellar structure were slices as given in Fig. 1b.The phase structure of EG and SGFs were characterized by XRD

asshownin Fig.3. Thesharpandintensivediffractionpeaksat26.3 ,56.0 correspond to EG and SGFs, respectively. A third diffractionpeakofSGFsat45.0 appearedparticularlybecauseultrasonicmadestructure of graphite flake into disorder.

3.2. The composite PCM

TheSEM imagesof binarymolten salts andcomposite PCMsam-ples were shown in Fig. 4. As shown in Fig. 4a, the NaNO3KNO3eutecticcrystalwasgraymilkysubstancewhichlookedlikesmoothblock. The images in Fig. 4be correspond to samples with EG

at mass rates of 0.5, 1.0, 1.5, 2.0%, respectively. Judging from theimages, we might draw the conclusion that SGFs were well dis-persed in eutectic crystal with foliated and angular structure.

The phase structure of molten salts and composite PCM sam-ples were characterized by XRD at room temperature as shownin Fig. 5. The peaks at 26.3, 56.0 correspond to SGFs. However,the weak feature peak of SGFs centered at 45.0 completely disap-pears after the compositePCM composed.The peaks at 23.0,28.5,38.0 correspond to potassiumnitrate andthe peaks at 31.5, 46.0,47.5 correspond to sodium nitrate, respectively. Obviously, potas-sium nitrate and sodium nitrate were the main crystal phases asidentified in Fig. 5(a). Further, the position of peaks was withoutexcursion which proved that the phase structure of nitrate crys-tal were no chemical reaction. Due to the little additive of EG, its

presentation was unobvious in the composite PCM.The chemical composition of the prepared composite PCM wasfurther determined by EDX analysis attached to the SEM. The EDXspectrum (Fig. 6b and c) sustains that the composite PCM (Fig. 6a)consists of C, N, O, Na and K elements. The strong N, O, Na andK signal originates from binary nitrates, while the C signal comesfrom the EG. Whats more, the difference of percentage content ofC in the two samples (Fig. 6b and c) was caused by mutual interfer-ence of C and K element belonging to low atomic sequence and thelittle quality of test samples, etc. According to the above analysis,it is unambiguously demonstrated that EG had been successfullycombined into binary nitrate crystal.

The images of map scanning in Fig. 7bf correspond to C, N,K, Na, and O elements attached to the SEM (Fig. 7a), respectively.

The dispersion of every element in samples could be easily judged.


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54 J. Xiao et al. / Thermochimica Acta 587 (2014) 5258

Fig. 1. Scanning electron microphotographs of (a) EG and (b) SGFs by coating conditionat room temperature.

Fig. 2. Transmission electron microscope of SGFs from different angles at room temperature.

The white spots presented homogeneous distribution of C elementin Fig. 7b and a white reunion was found in top-right corner. Thereunionwasformedbecausemutualinterferencebetweenthelightelements,the littlequantityof measured samples andthe influenceof different area, etc.

The specific heat, thermal diffusivity and thermal conductivitycoefficient of composite PCM have had variations under the effectof SGFs. These parameters of the PCM samples have been mea-sured at room temperature as listed in Table 1. As the increasing

addition of EG, it could be seen that specific heat increased firstsharply and then slowly, however, thermal diffusivity and ther-mal conductivity coefficient increased almost linearly. As shown inTable 1, the specific heat of sample with 2.0 wt.% EG is 2.600 J/(gK),thermaldiffusivityis0.930mm2/s, thermal conductivity coefficientis 4.884 W/(mK), which correspond to 1.11 times, 1.95 times, 2.15times than that of binary molten salts. The results proved that EGhad greatcontribution to thermal conductivity coefficient of binarymolten salts which was in accord with the report in Xiaos paper

Fig. 3. X-ray diffraction pattern obtained forEG and SGFs at room temperature.


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Fig. 4. The SEM images of binarymolten saltand composite PCM samples at room temperature.

Table 1

The specific heat, thermal diffusivity and thermal conductivity coefficient ofsamples.

No. EG (wt.%) Specific heatJ/(g K)

Thermal diffusivity(mm2/s)

Thermal conductivitycoefficient W/(mK)

1 0 2.351 0.477 2.272012 0.5 2.485 0.573 2.8763 1 2.586 0.639 3.3384 1.5 2.593 0.791 4.1435 2 2.6 0.93 4.884

[30]. The enhancementof thermal conductivity coefficient couldbeexplained as following:

(1) According to the formula: =c, represents thermalconductivity coefficient, representsthermaldiffusivity, rep-resents density, c represents specific heat. Due to the closedensity of graphite and binary molten salts and the little

addition of EG, the impact of density on thermal conductivitycoefficient could be ignored.

(2) During the preparation, SGFs were well dispersed into binarymolten salts afterultrasonic. As molten saltscrystallizing, thereis certain crystallizing pressure which excludes SGFs to thegrain boundary surface. Then the very complex meshes areformed by graphite slices which couple with molten salts. Asa result of its distinct thermal properties, the graphite is equiv-alent to small high conductive transport channels for heatconduction and also overcome the interface thermal resistanceto a certain extent. Consequently, thermal conductivity coeffi-cient of the composite PCM is improved significantly.

As to thephasechange characteristics, thephasetransition tem-perature and latent heat were measured by DSC. The DSC curves ofbinary molten salt and composite PCM samples at room tempera-ture were presented in Fig. 8. The peak temperatures, latent heatand other parameters were listed in Table 2. It should be noted

Fig. 5. X-ray diffraction pattern obtained for binary moltensalt and composite PCM at room temperature.


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Fig. 6. The X-ray energy spectrum curves of a composite PCM sample.

Fig. 7. Map scanning of a composite PCM sample.

Table 2

Theparameters of phase changetemperature and latent heat of samples.

No. EG (wt.%) Solidsolid phase change Solidliquid phase change Total latent heat (J/g)

Peak temperature (C) Latent heat (J/g) Peak temperature (C) Latent heat (J/g)

1 0 130.6 17.26 223.2 142.2 159.462 0.5 130.1 19.95 225.6 128.7 148.653 1 130.4 18.69 224.8 128.4 147.094 1.5 130.0 18.71 224.7 128.1 146.815 2 130.2 17.51 225.3 124.4 141.91


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Fig. 8. DSC curves of binarymolten salt and composite PCM samples.

that every curve had two transformation peaks and the peaks werematched nearly at same temperatures. These results nearly corre-spond to the DSC profiles of the mixture of NaNO3and KNO3[32].Concluding from the analysis of XRD and SEM, the peak at about130.4 C was formed by solid-solid phase change and the peak atabout 224.8 C was formed by solidliquid phase change.

The fluctuation of phase transition temperatures was veryinsignificant and reduction on the total latent heat of compositePCM (PTLH) was slight, as compared to binary molten salt corre-spondingly. The reduction on the total latent heat of compositePCM (PTLH) was calculated by comparing to the total latent heat ofbinary molten salt (BTLH). A non-dimensional parameter formu-lated as Eq. (1) was used for presenting the reduction percentageon the total latent heat of composite PCM to binary molten salt.

= (BTLH PTLH)BTLH (1)

It can be drawn from Table 2 that reduction percentage onthe total latent heat was about 6.7811.01%. According to Table 2,it could also be known that the solidsolid phase change whichaccounted for about 10% total latent heat had the relatively smallvariations and the solidliquid phase change had a major contribu-tion to total latent heat. The total latent heat of binary molten saltsample has obvious difference with that of composite PCM sam-ples, butresults of compositePCM samples have similar latentheat.This phenomenon could be explained that the addition of EG hasreduced the mass rate of binary molten salt without contributiontotal latent heat and influenced PTLH little by the same pattern.The results of our samples had no difference to that in previous

researches [2730]. From what has been discussed above, it couldcometoaconclusionthatEGhadlittleinfluenceonphasetransitionand total latent heat of the composite PCM.

4. Conclusion

Based on the above results, the nitrate salts/EG composite PCMshows an excellent thermophysical performance as a heat transferand energy storage material. The composite PCM was prepared viaadding different mass rate of EG to binary nitrate salts consistingof NaNO3 and KNO3 (6:4) by aqueous solution method adoptingultrasonic.

The investigated morphology and thermo physical propertiesshowed SGFs were well dispersed and homogeneous distributed

in eutectic crystal with no chemical reaction after ultrasonic. As

the increasing mass rate of EG, it could be seen that specific heatincreased first sharply and then slowly, however, thermal diffusiv-ity and thermal conductivity coefficient increased almost linearly.It can be indicated that EG have given a great rise to thermalconductivity coefficient which largely increased to 4.884W/(mK)and a nearly 11.0% reduction to latent heat. During the tests, wecan conclude that the melting curves contain two phase change:solidsolid phase change and solidliquid phase change. Thefluctuation of phase transition temperatures was very insignificantand the total latent heat of composite PCM had a reduction about6.7811.01%. In general, the nitrate salts/EG composite PCMis suitable for heat transfer and thermal energy storage as EGenhanced the thermal conductivity of binary nitrate salts.

Acknowledgements

The authors would like to express their sincere thanks to thefinancial support from the National Natural Science Foundation ofChina (Grant no. 51006024), the Special Funding of Combinationof Production, Teaching and Research of Guangdong Provincial andNational Ministry of Education (Grant no. 2011B090400446), theSpecial Funding of discipline construction of Guangdong Province

(Grantno. 2012KJCX0041), andthe Special Funding of applied basicresearch of Guangzhou City (Grant no. 2013J4100010).

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