diamond ethylene glycol-nanofluids for solar energy applications

Accepted Manuscript Graphite/diamond ethylene glycol-nanofluids for solar energy applications E. Sani, N. Papi, L. Mercatelli, G. Żyła PII:

S0960-1481(18)30389-6

DOI:

10.1016/j.renene.2018.03.078

Reference:

RENE 9947

To appear in:

Renewable Energy

Received Date: 22 November 2017 Revised Date:

5 March 2018

Accepted Date: 28 March 2018

Please cite this article as: Sani E, Papi N, Mercatelli L, Żyła G, Graphite/diamond ethylene glycolnanofluids for solar energy applications, Renewable Energy (2018), doi: 10.1016/j.renene.2018.03.078. This is a PDF file of an unedited manuscript that has been accepted for publication. As a service to our customers we are providing this early version of the manuscript. The manuscript will undergo copyediting, typesetting, and review of the resulting proof before it is published in its final form. Please note that during the production process errors may be discovered which could affect the content, and all legal disclaimers that apply to the journal pertain.

ACCEPTED MANUSCRIPT

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Graphite/diamond ethylene glycol-nanofluids for solar energy applications

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E. Sani1*, N. Papi1, L. Mercatelli1, G. Żyła2

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CNR-INO National Institute of Optics, Largo E. Fermi, 6, I-50125 Firenze, Italy Department of Physics and Medical Engineering, Rzeszow University of Technology, 35-905 Rzeszow, Poland * Corresponding author: [email protected]

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Abstract The rapid development of thermodynamic solar systems requires increasingly efficient absorption materials. This work reports on the investigation of light-intensity dependent optical properties of graphite/nanodiamond suspensions in ethylene glycol, in the perspective to evaluate their potential for direct absorption solar collectors and solar vapor generation. The study was carried out two sample types, differing in the ash content (0.3% and 5.9% wt in the powder), and at three concentrations each (0.0025%, 0.0050%, 0.0100% wt in the fluid). A high sunlight extinction was found, with full absorption in 15 mm and 30 mm path lengths for the 0.0100% and 0.0050% wt concentrations, respectively. This makes investigated nanofluids appealing as volumetric direct solar absorbers in solar collectors. Moreover, by characterizing optical properties at high incident intensities, we proved the creation of vapor bubbles in the base fluid via optical limiting effects active at least from ultraviolet to near infrared wavelengths. This result propose graphite/nanodiamond-based suspensions for sunlight-induced vapor generation application as well.

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Keywords: Carbon, graphite, nanodiamond, nanofluids, optical properties, solar energy, optical limiting.

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Introduction

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Conventional solar collectors operating at low-mid temperatures consist of a sunlight

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absorbing coating deposed on a solid surface which exchanges heat with a working fluid.

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Energy losses due to thermal re-radiation by the heated absorber are typically reduced by

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a vacuum insulation of the absorbing surface. This scheme can be significantly simplified

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by the use of a dark fluid working both as volumetric light absorber and heat exchanger.

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In 1975 was launched the first idea of a direct-absorption solar collector (DASC) using a

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black liquid [1]. However, the India ink-based fluid investigated in that work was not 1

ACCEPTED MANUSCRIPT suitable, being subject to thermal and light-induced degradation. Thus the idea was

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substantially abandoned for many years, until the development of nanotechnology

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allowed the production of new nanoparticle-loaded fluids with superior stability

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properties [2-8]. To date, a large number of nanomaterials have been investigated in this

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sense, including metallic nanoparticles, insulating oxides as alumina, titania [9], silica,

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semiconductors as zinc oxide [10], and many others [5, 11-16]. Among the investigated

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materials, the family of carbon-based nanostructures has emerged as particularly

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promising. From carbon black [7] to graphite [5, 17], as well as carbon nanostructures

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(e.g. single-wall, multi-wall and functionalized nanotubes [5, 18-20], carbon nanohorns

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[3, 6, 7, 21], graphene and graphene oxide [22, 23]), many nanofluids containing

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nanoparticles of carbon allotropes have been proposed for solar energy applications.

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A second promising field of application of nanofluids in renewable energies is direct solar

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steam generation. Steam production is of crucial importance for many applications

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including electricity generation, energy storage, water desalination and sterilization [24-

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26]. Green and renewable steam production by solar energy is thus an important topic of

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research [27], as an example in order to bring technologies essential for life in off-grid

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areas and resource-poor locations. Typical solar steam production systems are currently

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based on solar trough or solar tower architectures with a surface or cavity solar absorber

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[28-30]. They work heating a bulk fluid to its boiling temperature under high optical

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concentration. The steam generation efficiency is strongly connected to the surface

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temperature and thermal radiation properties of the absorber. However as bulk steam

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production needs high temperatures, these conventional systems also suffer from high

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heat losses and low efficiency. To overcome this drawback, a possibility is looking for

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solutions able to produce steam without requiring heating the whole liquid volume to the

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boiling point. Different Authors reported on the efficient solar steam generation by

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different nanoparticles, such as gold [31-33], silicon [34] and carbon nanostructures [35,

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36].

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Nanodiamond-based nanofluids have received a great interest in last years. However,

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while thermal, electrical and tribological properties have been extensively characterized

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[37-55], the knowledge of their optical properties remains quite scanty, except for their

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fluorescence properties in presence of impurities and defects [56, 57], which were

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investigated mainly for biological applications [58, 59].

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ACCEPTED MANUSCRIPT In this work, we report on the characterization of optical properties of two

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graphite/nanodiamond suspensions in ethylene glycol for DASC applications. In addition,

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we also investigated the nanofluid response to high intensity laser radiation, to evaluate

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the potential of these nanoparticles for direct solar vapor generation. It should be noticed

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that our suspensions are based on ethylene glycol, however the obtained results can be

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extended to aqueous suspensions as well.

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Experimental

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Nanofluids have been prepared by dispersing commercially available nanopowders

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(PlasmaChem GmbH, Berlin, Germany) in ethylene glycol. Two types of nanopowders

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were used; both of them were mixtures of graphite and nanodiamonds (ND) with ND

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phase over 26% as declared by the producer, and differing each other as for the ash

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content. In the following, samples with higher (5.9%) and lower (0.3%) ash fractions will

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be labeled as ND1 and ND2, respectively.

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Before suspending them in the fluid, physico-chemical properties of nanopowders were

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evaluated by X-ray diffraction (XRD) (Bruker D8 Advance, Bruker GmbH, Karlsruhe,

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Germany) and SEM coupled to energy dispersive X-ray spectroscopy (EDS) (JEOL-JSM-

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6301F, JEOL USA Inc., Peabody, USA). Results of those measurements are shown in

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Figure 1. In the EDS investigation of sample ND1 (inset in Fig. 1A), spherical particles

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containing Fe and O are clearly visible, while sample ND2 contains mostly carbon as

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expected (inset in Fig. 1B). XRD (Fig. 1C) confirms that both powders contain graphite

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and diamond phases and that ND1 contains maghemite Fe2O3. Detailed discussion on the

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powder characterization is reported in Ref. [55].

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Figure 1. a) EDS spectra analysis of nanopowders with 5.9% ash (ND1); b) EDS spectra

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analysis of nanopowders with 0.3% ash (ND2); inserts presents EDS images of sample

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areas under investigation. c) XRD diffractogram of nanopowders. Reprinted with

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permission from Ref. [55]. 4

ACCEPTED MANUSCRIPT The first step of the nanofluid preparation was measuring the mass of nanoparticles on

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analytic balance WAS 220/X (Radwag, Radom, Poland). Then ethylene glycol was added

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and the sample was mixed for 30 minutes in Genius 3 Vortex (IKA, Staufen, Germany).

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After that, ultrasounds were used for 200 minutes in an Emmi 60 HC bath (EMAG,

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Moerfelden-Walldorf, Germany), to break agglomerates of nanoparticles. Figure 2 shows

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a photo of the samples at the mass concentrations investigated in present work.

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Figure 2. Photo of samples studied in the present work and comparison with the pure ethylene glycol (EG).

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Spectral optical transmittance in the linearity regime has been measured using a double-

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beam UV-VIS spectrophotometer (PerkinElmer Lambda900) using a variable length cell

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[60, 61]. High intensity light irradiation experiments have been carried out using a pulsed

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nanosecond Nd:YAG laser as light source (Quantel Q-smart 850, delivering 6 ns pulses at

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1064, 532 and 355 nm wavelength). The three laser emission wavelengths were spatially

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separated by proper optical elements and focused on the sample by a lens of 300 mm

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focal length. The sample was held in a quartz cuvette with 10 mm path length, put in a

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defocused position to avoid cuvette damage. The beam exiting the sample was collected

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by a couple of lenses of focal lengths 40 and 100 mm and focused on a pyroelectric

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detector (Ophir PE25C). The energy incident on the cuvette could be varied by means of

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proper polarizer beam splitters and measured using a pyroelectric detector (Ophir

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ACCEPTED MANUSCRIPT PE50BE) (Figure 3a,b).

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Figure 3: a) Photo and b) Scheme of the experimental setup for optical limiting experiments. L1, L2, L3: lenses; BS: beam splitter; Ein: input energy measurement; Eout: output energy measurement.

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Results

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Optical properties at low input intensity

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Three concentrations (0.0025%, 0.005% and 0.01% wt) were investigated for each

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sample. Figure 4 compares the transmittance spectra of nanodiamond suspensions ND1 6

ACCEPTED MANUSCRIPT and pure base fluid for 2 mm path length. The sunlight spectral irradiance is also reported

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for reference. The addition of nanodiamonds considerably decreases the transmittance of

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the fluid with respect to the pure glycol, with a major effect on the spectral region where

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sunlight emission is higher. This result opens interesting perspectives for the use of these

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nanofluids as volumetric solar absorbers.

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Figure 4: Transmittance spectra of nanodiamond-nanofluids and comparison with the transmittance of the pure glycol. Sunlight spectral irradiance is also superimposed for reference (pink curve).

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If the difference between the two samples is concerned, in the spectral range 300-2300

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nm no significant differences could be detected for fixed concentration (Figure 5)

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Extinction coefficient (cm-1)

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Concentration 0.005% wt 60

ND1 ND2

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Wavelength (nm)

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Figure 5: Comparison of the extinction coefficient of the two samples at the same 0.005% wt concentration.

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The obtained extinction coefficient of nanofluids allowed assessing good sunlight

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extinction characteristics even with very low nanoparticle concentrations, with promising

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potential in DASC application. For a comparative evaluation, an useful quantity to define

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is the extinct energy fraction EF, at the propagation length x within the fluid [6]

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EF ( x ) = 1 −

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∫ λ

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where I(λ) is the sunlight spectral irradiance [62], µ(λ) is the spectral extinction

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coefficient, λmin= 300 nm and λMAX=2600 nm.

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Figure 6: Sunlight extinction as a function of the propagation length within the fluid.

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Figure 6 compares the calculated EF(x) fraction for pure glycol and for the nanoparticles

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concentrations of 0.005% and 0.01% wt. As observed above, the addition of nanoparticles

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considerably improves the light extinction capability of the fluid, arising in the full light

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extinction in about 15 or 30 mm, for 0.01% and 0.005% concentrations, respectively. It

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should be noticed that our investigated concentrations are very low. However, as the

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extinction coefficient increases with the concentration, the propagation length to achieve

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100% sunlight extinction can be set at a desired value by simply tuning the nanoparticle

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load in the fluid. As a second comment, we underline that present measurements are

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concerned with the extinction coefficient, which includes both the contributions of light

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absorption and light scattering. Even if the light scattering effect is difficult to evaluate in

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our case, as nanoparticles are constituted by a multi-modal size distribution with both

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nanodiamond

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graphite/nanodiamond-nanofluids show a potential for DASC applications already at the

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investigated low mass fractions. Finally, it can be important to note that, thanks to the low

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nanoparticle amount needed, the increase in price with respect to the bare ethylene glycol

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is low, making these nanofluids fully affordable from the economical point of view. For

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reference, for laboratory-scale supplies the price increase was only about 0.10-0.50 Euro

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per liter of nanofluid. A consistent price reduction can be expected from economy of

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and

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scale, making thus the price increase of nanofluid with respect to the pure fluid almost

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negligible.

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Optical properties at high input intensity

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Before presenting the results of experiments at high input light intensities, it is useful to

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give a brief introduction of the phenomenon of optical limiting (OL). OL helps to explain

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the obtained data in terms of generated bubbles within the fluid (see below), assessing the

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sample potential for vapor generation as well.

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OL is an example of nonlinear optical behavior. In particular, a material is said to show

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OL when its optical response depends on the input light intensity as follows: at weak

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input intensities, the light transmitted through the material linearly depends on the

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intensity of incident radiation. In these conditions, the value of optical transmittance is

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constant and independent on the input light intensity. However, when the intensity of

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input light becomes higher than a threshold value characteristic of the material, the

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intensity of transmitted light turns in a dependence less than linear on the input light,

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becoming also, in ideal cases, constant and independent on the incident intensity. In this

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regime the transmittance suddenly decreases with respect to its initial low-intensity value,

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reaching, for high input intensities above threshold, values even near to zero. In these

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conditions, the material becomes opaque or near-opaque to the incident high-intensity

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radiation. Even if the detailed study of OL is beyond the scope of the present work, it

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should be anyway mentioned that OL is important for many application fields e.g. optical

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communications, optical computing, security, military, laser protection etc and, basically

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speaking, in all fields where the efficient manipulation of optical beams is required.

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Figure 7 shows the normalized transmittance (i.e. the ratio between output and input

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energy, normalized to its value in the linearity regime) as a function of the input laser

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fluence for the two samples ND1 and ND2, for the same 0.005% concentration.

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1064 nm 532 nm 355 nm

1.0 0.9 0.8

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Normalized transmittance Eout/Ein

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Figure 7: Optical limiting performances of a) ND1 and b) ND2, at 0.005% wt concentration. Values around unity of normalized transmittance indicate the subsistence of linear regime, while decreasing transmittance values versus input fluence demonstrate the nonlinear behavior.

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For both samples a dramatic nonlinear behaviour has been demonstrated at all the three

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investigated wavelengths (Figure 7). Nonlinearity is stronger at short wavelengths, in

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agreement with the higher linear extinction coefficient (see Fig. 5). It is interesting to

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observe that the samples did not show any degradation after many iterations of high-

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intensity experiments. This confirms the high stability of these nanofluids. 11

ACCEPTED MANUSCRIPT The appearance of OL in nanosuspensions basically can be explained by two

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mechanisms: nonlinear absorption or nonlinear scattering [63], depending on the nature of

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nanoparticles and on the properties of the suspending fluids [64]. Which is the effect

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actually occurring can be identified applying semi-empirical models. Nonlinear

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absorption can be due to different effects like reverse saturable absorption, two-photon

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absorption etc [64]. It can modeled introducing a nonlinear term in the Lambert-Beer law

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[65]:

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()



= − − ħ  (1)

where F(z) is the energy fluence at the z position in the sample, is the linear extinction

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coefficient,  is the Excited State Absorption (ESA) cross section. If this equation is

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solved following the method described in [65, 66] the output energy Eout is linked to the

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incident energy Ein according the relationship:

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      ⁄$

  = !". 

(2)

Where &' is a coefficient describing reflection losses on the cuvette walls and L is the

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sample thickness. The term ( )* describes the linear extinction, and  is the threshold

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energy defined as the energy where the transmittance decreases to the 90% of its original

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value [65].

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On the other hand, a model where OL is only due to nonlinear refraction has been

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developed in [67]. In the cited reference, nonlinear properties are ascribed to nonlinear

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scattering between lasers photons and vapor bubbles yielded by ionization and

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vaporization of the nanoparticles and/or by the vaporization of the base fluid:

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.



 .

 =  ( )* +1 +  /  − 101 $

(3)

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where αe is the nonlinear extinction coefficient and Et is the energy threshold for bubble

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formation and are obtained from a fitting procedure of experimental data.

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In Figure 8, the results of data fitting with Eqs. (2) and (3) for sample ND2 at the

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concentration of 0.005% and at 532 nm wavelength are shown. The linearity regime is

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also reported in the graph for comparison (green line). It is possible to appreciate how the 12

ACCEPTED MANUSCRIPT nonlinear scattering in Eq. 3 well reproduces the experimental behavior, clearly showing

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the role of bubble formation in explaining the observed nonlinearity, while the fitting with

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Eq. 2 is much less satisfactory. Different combination of sample type/concentration/ laser

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wavelengths allowed obtaining the same result. In agreement with that observed for

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carbon nanotubes and for some kind of nanodiamonds in water, but at higher energies

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than those investigated in the present work [68], we can attribute the nature of bubbles to

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heat transfer from the nanoparticle to the surrounding base fluid, inducing the

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vaporization of the fluid itself and the growth of the bubble [69].

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Figure 8: Experimental data fitting for sample ND2, 0.005%wt concentration, 532 nm wavelength

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As for the dependence of OL from the concentration, we obtained that for both samples,

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OL is more efficient at higher concentrations, similarly to what reported for carbon

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nanotubes [70] and gold nanoparticles [71].

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In summary, we demonstrated bubble generation in graphite/nanodiamond suspensions in

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ethylene glycol at 355, 532 and 1064 nm wavelength, with no significant differences

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among ND1 and ND2-type samples. The investigated wavelengths span the spectral range

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of highest intensity of solar radiation. Thanks to the spectrally broadband light extinction 13

ACCEPTED MANUSCRIPT characteristics of our samples (Figure 5), we expect that the evidenced bubble generation

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is not spectrally-selective at all and can be induced by a broadband source like sunlight as

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well. The involved energy fluences (0.1÷0.8 J/cm2, Figure 7), at 10 Hz laser pulse

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repetition rate, are compatible with solar concentration systems [72]. Moreover, as

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mentioned above, the suspensions were very stable and did not show sedimentation and

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degradation issues after high-intensity measurements, differently from other carbon

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nanoparticles [73]. Therefore the obtained results show that graphite/nanodiamond

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nanofluids are promising for solar vapor generation and solar desalination applications. In

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fact, the literature already reports on the successful suspension of nanodiamonds in water

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[38, 39, 52, 68] and there are no reasons to expect that this task for nanodiamonds would

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be more difficult than for other carbon-based nanostructures [6, 74].

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Conclusions

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In this work, suspensions of graphite/nanodiamond nanoparticles in ethylene glycol were

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prepared and characterized. Spectrally-resolved linear optical properties showed a

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significantly lower transmittance than pure base fluid, arising in a high sunlight

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absorption of these nanofluids with promising potential in direct-absorption solar

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collectors. Analyzing the optical limiting performances at three wavelengths in the UV,

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visibile and near infrared range we demonstrated the generation of vapor bubbles around

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nanoparticles at light intensities comparable to sunlight concentration systems, thus

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showing the promising potential of graphite/nanodiamond mixures for solar vapor

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generation and desalination as well.

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Additional material

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Video recording of bubble generation for sample ND1 at the concentration 0.01% wt and

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1064 nm wavelength.

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Acknowledgments

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This research was carried out under the auspices of EU COST Action CA15119:

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Overcoming Barriers to Nanofluids Market Uptake (NANOUPTAKE). The Italian bank

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foundation “Fondazione Ente Cassa di Risparmio di Firenze” is gratefully acknowledged 14

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(pratica n. 2015.0861). Thanks are due to Mr. M. D’Uva and Mr. M. Pucci (CNR-INO)

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for technical support and to Mrs. Roberta Parenti, Mrs. Pasqualina Pipino and Mrs. Ilaria

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Bini (CNR-INO) for administrative support.

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ACCEPTED MANUSCRIPT Highlights

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Nanofluids consisting of graphite/diamond nanoparticles in ethylene glycol have been prepared
We studied optical properties in the linearity regime
We found a considerable sunlight extinction even with low nanoparticle loading
Optical properties were then assessed at higher light intensity
We proved direct vapor generation under irradiation at 355, 532 and 1064 nm