Photothermal investigation of poly (3-hexylthiophene): ZnSe nanocomposites

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Applied Physics AMaterials Science & Processing ISSN 0947-8396 Appl. Phys. ADOI 10.1007/s00339-015-8995-5

Photothermal investigation of poly (3-hexylthiophene): ZnSe nanocomposites

Dhekra Loubiri, Zied Ben Hamed,S. Ilahi, A. Sanhoury, F. Kouki &N. Yacoubi

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Photothermal investigation of poly (3-hexylthiophene):ZnSe nanocomposites

Dhekra Loubiri • Zied Ben Hamed •

S. Ilahi • A. Sanhoury • F. Kouki • N. Yacoubi

Received: 3 August 2014 / Accepted: 12 January 2015

� Springer-Verlag Berlin Heidelberg 2015

Abstract Optical and thermal properties of poly (3-hex-

ylthiophene): ZnSe blend thin films with different mass

ratio of ZnSe nanoparticles (NPs) are investigated by the

photothermal deflection technique. The optical absorption

spectra and the sub-band gap energy are evaluated by

comparing the experimental and the theoretical PDS sig-

nals amplitude. The thermal parameters are estimated by

fitting the PTD data. The ZnSe NPs dependency with these

parameters has been shown. In fact, it was found a redshift

of the sub-band gap energy behavior and a decrease in both

thermal conductivities as and thermal diffusivities with the

increase in NPs concentration in polymer matrix at low and

medium mass ratio. The opto-thermal parameter variations

are attributed to the effect of the mass ratio between

polymer and ZnSe NPs.

1 Introduction

The alloy of conjugated polymers with inorganic semi-

conductor nanoparticles is a new generation of organic

semiconductors in order to improve some characteristics of

the conjugated polymers [1–5].

Emitting diodes (LEDs) based on the bulk heterojunc-

tion (BHJ) are one of the most attractive studies thanks to

their several advantages such as light weight, flexibility,

low cost and simple fabrication with large processing area.

Various strategies have been used to improve the efficiency

of these devices, including the tandem architecture [6, 7].

Recent studies have reported the effects of ligand-

exchanged nanoparticles and polymer [8–10]. However, the

problem in the above devices lies in the fact that NPs in the

polymer matrices are highly unstable and have higher ten-

dencies of agglomeration, which leads to their nonhomo-

geneous dispersion in polymer matrices [11]. Besides this, it

has also been reported [12] that the surface passivating

ligand affects the quality, stability and photooxidative nat-

ure of the surfaces of the NPs and hence plays a significant

role in influencing the properties of their polymer nano-

composites. Interesting studies have been conducted on the

incorporation of NPs zinc selenide: ZnSe in the polythio-

phene. Indeed, ZnSe NPs or ZnSe quantum dots (Qds)

materials have attracted a considerable attention during the

past decade due to their remarkable optoelectronic, mag-

netic and electrical properties [13–15]. Furthermore, there

are two kinds of excitons in the nanocomposite: the Frenkel

exciton in the organic materials, and the Wannier–Mott

excitons in inorganic materials. Nanocomposite excitons

have the properties of both types of excitons, and they are

very sensitive to external perturbations or varying in per-

centage weights [16]. The most important mechanisms are

the exciton capture by NPs in a polymer matrix [17].

D. Loubiri (&) � S. Ilahi � N. Yacoubi

Unite de Recherche de Caracterisation Photothermique & Bruit

dans les Composants, Institut Preparatoire aux Etudes

d’Ingenieurs de Nabeul (IPEIN), Universite de Carthage,

8000 Merazka, Nabeul, Tunisie

e-mail: [email protected]

Z. Ben Hamed � F. Kouki

Laboratoire, Materiaux avances et phenomenes quantiques,

Faculte des Sciences de Tunis, Universite de Tunis El Manar,

Campus Universitaire, 2092 Tunis, Tunisie

A. Sanhoury

Laboratoire de Chimie Organique Structurale, Synthese et

Etudes Physicochimiques, Faculte des Sciences de Tunis,

Universite de Tunis El Manar, Campus Universitaire,

2092 Tunis, Tunisie

F. Kouki

Institut Preparatoire aux Etudes d’Ingenieur El-Manar,

Universite de Tunis El Manar, Campus Universitaire,

2092 Tunis, Tunisie

123

Appl. Phys. A

DOI 10.1007/s00339-015-8995-5

Author's personal copy

The nanocomposite P3HT: % ZnSe presents a promis-

ing area in the LEDs application as shown by Mastour et al.

[18]. The increase in percentage weights leads to an

increase in the fluorescence intensity. This result shows the

importance of the optical absorption spectrum study of

these nanocomposites in order to deduce the band gap

energy.

This work describes an experimental investigation of the

ZnSe NPs concentration effects on the optical and thermal

properties variations of P3HT thin films by the photother-

mal deflection technique (PTD).

2 Theory

The PTD is a sensitive optical tool for material analysis

[19]. The principle of PTD technique is shown in Fig. 1.

The sample is heated by a modulated light beam which

generates a thermal wave that propagates into the sample

and surrounding media, inducing a refractive index gradi-

ent in the fluid that causes the deflection of a laser probe

beam skimming the sample surface. The deflection is

proportional to the complex temperature T0 at the sample

surface. As the incident light is assumed to be uniform and

only the sample absorbs the light with an absorption

coefficient a, a one-dimensional treatment of the thermal

wave is sufficient.

The obtained surface temperature T0 is given by the

following equation [20]:

Where b ¼ Kbrb

Ksrs; r ¼ a

rs; g ¼ Kfrf

Ksrs; ri ¼ ð1þjÞ

li; li ¼

ffiffiffiffi

Di

pf

q

, a

is the optical absorption coefficient of the hybrid layers, f is

the modulation frequency, and h is thickness of the hybrid

layer. Ki, Di and li are, respectively, the thermal conduc-

tivity, the thermal diffusivity and the thermal diffusion

length of the i medium. Here, the index i takes the sub-

scripts s, f and b, respectively, for the sample (hybrid

layer), fluid (paraffin oil) and backing. The thermal diffu-

sivity and thermal conductivity of paraffin oil and Plexiglas

are reported in Table 2.

The expression of probe beam deflection is [20]:

W ¼ L

n

dn

dTrfT0 expð�rfx0Þ ð2Þ

Where n is the refractive index, and L is the sample length in

the direction of the laser probe beam. Here, W is a complex

number which can be written as W ¼ Wj j expðuÞ where Wj jis the amplitude and u the phase; x0 is the distance between

the probe beam axis and the sample surface.

3 Experimental details

3.1 NPs synthesis and layer deposition

Zinc selenide NPs were prepared following a method

described by Khanna et al. [21] with some modifications

using tributylphosphine (TBP) instead of trioctylphosphine

derivatives in order to reduce the bulkiness of the capping

agent; a 1:1 mixture of anhydrous zinc acetate and oleic

acid in diphenyl ether (30 mL) was refluxed at 140 �C for

2 h. To this solution was added an appropriate quantity of

tributylphosphine selenide (TBPSe) in tributylphosphine

(5 mL). The reaction mixture was heated at 180 �C over-

night. Methanol was added to the yellow suspension

obtained to cause further precipitation. The suspension was

centrifuged three times at 4,000 rpm for 30 mn followed by

washing with hexane and drying in an oven to obtain ZnSe

as yellow powder. The nanoparticles have an average size

of 4–5 nm, which is consistent with the result obtained from

XRD data and calculated from Scherrer’s formula where the

Fig. 1 Schematic representation of the PTD principle

T0 ¼aI0

2Ke a2 � r2ð Þr � 1ð Þ bþ 1ð Þ exp rehð Þ � r þ 1ð Þ b� 1ð Þ exp �rehð Þ þ 2ðb� rÞ expð�ahÞ

gþ 1ð Þ bþ 1ð Þ exp rehð Þ � g� 1ð Þðb� 1Þ expð�rehÞ

� �

ð1Þ

D. Loubiri et al.

123


nanoparticles have a diameter in the range 3–4 nm

depending on the 2-h value and the crystal plane [22].

Commercial P3HT polymer purchased from Sigma-

Aldrich was dissolved in chloroform (30 g/l). The solution

was stirred for 6 h at room temperature to increase the

solubility. A nanocomposite solution was then prepared by

adding different mass ratio of ZnSe NPs to the polymer

matrix, while the same polymer concentration was kept for

all films.

The mass of ZnSe nanoparticles could be estimated by

the fact that is equal to the factor 0, 0.1, 0.4 and 0.8 multiply

by the polymer P3HT mass. In this way, we obtained a

series of composite solutions P3HT: ZnSe corresponding to

the respective mass concentrations 0 wt % (pure polymer),

10, 40 and 80 % of total mass of the nanoparticles com-

pared to the P3HT mass used for each film.

After the preparation, the nanocomposite solution was

spin-coated (model WS-6400BZ-6NPP/LITE) onto ordin-

ary glass substrate cleaned by ultrasonic treatment for

20 min in acetone followed by ethanol and dried under a

stream of argon. Finally, the samples were dried at 100 �C

for 30 min. The final film thicknesses vary approximately

between 400 and 800 nm.

3.2 Photothermal deflection setup

The experimental photothermal deflection (PTD) setup is

described in detail elsewhere [23, 24]. The sample is heated

by mechanically chopped light produced by a halogen lamp

of 100 W power. He–Ne laser probe beam of a 100 lm

diameter skimming the sample surface at x0 distance is

deflected. The deflection is detected by a position photode-

tector linked to a lock in the amplifier. The obtained photo-

thermal signal has two compounds: amplitude and phase. A

computer reads the values of amplitude and phase and draws

their variation versus square root modulation frequency.

However, for the photothermal deflection spectroscopy

(PDS), one can study the photothermal signal variations

versus wavelength, by incorporating a monochromator

between the halogen lamp and the sample. In order to

increase the sensitivity of the photothermal signal, the

sample was immersed in paraffin-oil-filled cell.

3.3 Morphological study

Investigations by optical microscopy image of hybrid lay-

ers are displayed in the Fig. 2.

The difference in contrast at different regions indicates

the presence of agglomerated ZnSe NPs. The images reveal

quite explicitly the heterogeneous distribution of ZnSe NPs

in P3HT matrix. Moreover, it is evident from Fig. 2 that

the aggregation of ZnSe NPs starts at sufficiently low

concentrations. The optical image of P3HT:10 %ZnSe

shows no aggregates of ZnSe NPs. However, as the con-

centration of ZnSe NPs increases, the size of the aggregates

rises up reaching tenths of micrometers.

Fig. 2 Optical microscopy

images of: a pristine P3HT,

b P3HT: 10 % ZnSe, c P3HT:

40 % ZnSe and d P3HT: 80 %

ZnSe

Photothermal investigation of poly (3-hexylthiophene)

123


ImageJ software allows determining the average

aggregate number. In fact, Fig. 3 shows that the average

aggregate formed increases with the weight percent of NPs.

Morphological evaluation of mixtures was made in a

previous study using SEM technique [22, 25] where the

authors of these papers have shown that there is a contrast

uniformity at low and medium mass ratio and a nonuniform

contrast for high values of the mass ratio. One notes also

that for high values of the mass ratio, there are not only

ZnSe IP aggregates that are visible, but also formation of

complexes.

4 Results and discussion

4.1 Experimental absorption spectra and gap energy

The experimental normalized photothermal signal’s

amplitude variations with respect to the wavelength in the

vicinity of the band gap energy of the P3HT: % ZnSe

hybrid layers presenting 10, 40 and 80 % ZnSe NPs con-

centration are depicted by the Fig. 4.

We notice that the amplitude presents two saturation

regions for high and low optical absorption coefficients and

exhibits a great sensitivity to the ZnSe NPs mass ratio in

the wavelength range between 580 and 680 nm. This var-

iation of the amplitude versus the ZnSe NPs mass ratio is

the result of band gap energy shift. In order to obtain the

optical absorption spectra, we have just to compare the

experimental normalized amplitude curves variation with

wavelength to the corresponding theoretical ones versus

optical absorption coefficient; thus, for a given values of a

normalized amplitude, one can affect for each wavelength

a corresponding optical coefficient as described in detail in

[26, 27].

The optical absorption spectra of P3HT: % ZnSe

nanocomposite layers are reported in Fig. 5. Indeed, these

layers exhibit a high absorption coefficient for wavelengths

(620–680 nm) which is in good agreement with photolu-

minescence experiments presented by Mastour et al. [18].

These curves permit to deduce the sub-band gap energy

of nanocomposites using Tauc’s law in the case of direct

band gap energy:

ðah#Þ2 ¼ bðh#� EgÞ ð3Þ

Where a is the absorption coefficient, h# is the photon

energy, Eg is the optical band gap, and b is energy-inde-

pendent constant with values between 105 and 106

cm�1eV�1 [28, 29].The presence of a slight displacement

is evident between the absorption edges of the films that are

related directly with the band gap energy variation.

Fig. 3 Average aggregates number versus the ZnSe NPs percentage

Fig. 4 Experimental amplitude of photothermal signal

Fig. 5 Absorption spectra of P3HT: wt% ZnSe NPs

D. Loubiri et al.

123


Figure 6 shows the graph of ðah#Þ2 versus h# for pristine

P3HT and P3HT: % ZnSe layers. The straight line portion

of the curve, when extrapolated to zero, gives the optical

sub-band gap energy.

The sensitivity of the PDS technique is localized in a small

range located in the immediate vicinity of the band gap

energy; thus, when the amplitude or phase of the photo-

thermal signal saturates, our technique becomes insensitive

to the variation of the optical absorption coefficient.

The band gap energy for the pristine P3HT, P3HT:

10 %ZnSe, P3HT: 40 %ZnSe and P3HT: 80 %ZnSe are

2.01, 1.92, 1.88 and 1.86 eV, respectively (Table 1).

One notes from these values that the band gap energy

decreases slowly with ZnSe mass ratio in the polymer

matrix.

Indeed, the optical behavior can be understood in terms

of an energetic disorder caused by the polymer morphology

[30, 31] as well as the incorporation of the ZnSe NPs.

Note that the shift of gap energy induced by the

polymer morphology change is of order of few meV [32].

In this system, the absorption band dependence in mass

ratio can be explained by the dispersion and the segre-

gation of ZnSe NPs into the P3HT matrix [25], as well as

the charge-transfer process [33]. In addition, the possi-

bility of polaron-related transitions present in our hybrid

layer can contribute to the sub-band gap shift as was

observed by A. Esser et al. and A. Kadashchuk et al. [34,

35]. By this fact, one believes that the increase in ZnSe

NPs mass ratio in the mixture causes an energetic disor-

der and a variation in the exciton migration in the hybrid

layers that may be attributed to the variation in the dif-

fusion length exciton.

5 Thermal properties

Thermal characterization of hybrid thin films is often a

non-trivial task due to the fact that polymer thermal

properties are very sensitive to the arrangement of the

molecules within. Thermal diffusivity value essentially

determines the rate of heat diffusion through the sample,

and the inverse of thermal diffusivity yields a measure of

the time required to establish thermal equilibrium in

systems for which a transient temperature change has

occurred. Even so, reports on the thermal conductivities

of these materials in thin films or device configurations

are limited.

Figures (7a, 8a) illustrate, respectively, the phase and

the amplitude of PTD signal versus square root of fre-

quency for the P3HT: % ZnSe nanocomposites. Indeed, the

phase and the amplitude present a different slope that

defined at each specimen its intrinsic thermal properties.

One notes that the slope decreases for the first three mass

ratios. Nevertheless, when the concentration of ZnSe NPs

is largely dominating (80 % ZnSe), the slope becomes

similar to the one of P3HT pristine.

On Figs. 7b–e and 8b–e are shown the experimental

curves fitted by the best theoretical ones. These coinci-

dences are obtained for given values, of thermal diffusivity

(D) and thermal conductivity (K) for each sample. The

details of multiparameters fitting are similar with that

described by Ref [36].

Knowing the values of K and D, one can deduce the

density and specific heat of the mixture: D ¼ KqC

� �

. One

notes that there is an increase in the product density and

specific heat with the ZnSe NPs mass. The obtained ther-

mal properties are reported in Table 2.

One sees that pristine P3HT presents the highest

thermal diffusivity and thermal conductivity values. For

the first three mass ratios, the incorporating of the ZnSe

NPs in the polymer matrix caused a reduction in its

thermal properties. This behavior can be ascribed to the

existence of interfacial thermal contact resistance

between the different constituent phases in a nanocom-

posite as well as their thermal expansion mismatch [37].

The existence of such thermal barriers results in a low-

ering of the thermal properties of the nanocomposite.

Fig. 6 ðaEÞ2 versus energy E near the band gap of P3HT: wt% ZnSe

NPs

Table 1 Gap energies of P3HT: ZnSe nanocomposites

Gap energy (eV) P3HT P3HT:

10 % ZnSe

P3HT:

40 % ZnSe

P3HT:

80 % ZnSe

PDS technique 2.01 1.92 1.88 1.86

PL technique

Ref. [18]

2.05 2.04 2.01 2.04


123


This can be explained by the growing up of the disorder

in the nanocomposites structures with ZnSe NPs

incorporation.

In contrast, the 80 % ZnSe NPs concentration presents a

thermal conductivity close to the pure P3HT. The crystal-

linity may play a large part in the thermal transport

Fig. 7 Phase of PTD signal versus the square root modulation

frequency, a experimental phase of the PTD signal according to

square root modulation frequency for P3HT: wt % ZnSe NPs,

b experimental (dots) and theoretical (line) phase of the PTD signal

for P3HT: 0 % ZnSe NPs, c experimental (dots) and theoretical (line)

phase of the PTD signal for P3HT: 10 % ZnSe NPs, d experimental

(dots) and theoretical (line) phase of the PTD signal for P3HT: 40 %

ZnSe NPs and e experimental (dots) and theoretical (line) phase of the

PTD signal for P3HT: 80 % ZnSe NPs

D. Loubiri et al.

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behaviors of these hybrid layers mainly for high concen-

tration of nanoparticles. When the concentration of ZnSe is

largely dominating, supersaturated nanoparticle clusters

grow on the top of the pores where further ripening occurs

via diffusion into and from the polymer network. Probably

the growing down of an interfacial thermal contact

Fig. 8 Normalized Amplitude of PTD signal versus the square root

modulation frequency, a experimental amplitude of the PTD signal

according to square root modulation frequency for P3HT: % ZnSe

NPs, b experimental (dots) and theoretical (line) amplitude of the

PTD signal for pristine P3HT, c experimental (dots) and theoretical

(line) amplitude of the PTD signal for P3HT: 10 % ZnSe NPs,

d experimental (dots) and theoretical (line) amplitude of the PTD

signal for P3HT: 40 % ZnSe NPs and e experimental (dots) and

theoretical (line) amplitude of the PTD signal for P3HT: 80 % ZnSe

NPs


123


resistance increases these thermal parameters in a sub-

stantial manner.

6 Conclusion

The effect of the ZnSe NPs concentration on optical and

thermal properties of a poly (3-hexilthiophene) thin film is

investigated by photothermal deflection technique. The

increase in ZnSe NPs mass ratio in the mixture causes an

energetic disorder and a variation in the exciton migration

in the hybrid layers that may be attributed to the variation

in the diffusion length exciton. However, thermal proper-

ties of our hybrid layers are found to be reduced compared

to pristine-conjugated polymer which is probably related to

the topology of the mixture that makes the interpretation of

the experimental results delicate since it tends to overes-

timate the expected ZnSe mass ratio derived from a simple

mixing model.

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Table 2 Thermal properties of

P3HT: ZnSe nanocompositesSamples Thermal diffusivity

(m2s-1)

Thermal conductivity

(W/m K)

Density

(g/cm3)

Specific heat

(104 J/Kg K)

Paraffin oil [38] 4 9 10-8 0.16

Plexiglas (backing) 0.2 9 10-6 0.1

Bulk ZnSe [39] 1.01 9 10-5 18.2

P3HT 3.522 9 10-7 1.782 1.33 0.3807

P3HT: 10 %ZnSe 0.987 9 10-7 1.043 1.46 0.7243

P3HT: 40 %ZnSe 0.179 9 10-7 0.250 1.86 0.7575

P3HT: 80 %ZnSe 0.249 9 10-7 1.964 2.39 3.3008

D. Loubiri et al.

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Photothermal investigation of poly (3-hexylthiophene): ZnSe nanocomposites

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