Shape and Size Effect on Photothermal Heat Elevation of Gold

Article Cite This: J. Phys. Chem. C 2019, 123, 17548−17554

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Shape and Size Effect on Photothermal Heat Elevation of Gold Nanoparticles: Absorption Coefficient Experimental Measurement of Spherical and Urchin-Shaped Gold Nanoparticles Hanane Moustaoui,† Justine Saber,† Ines Djeddi,† Qiqian Liu,†,‡ Amadou Thierno Diallo,† Jolanda Spadavecchia,† Marc Lamy de la Chapelle,†,‡,§ and Nadia Djaker*,†

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†

Université Paris 13, Sorbonne Paris Cité, UFR SMBH, Laboratoire CSPBAT, CNRS (UMR 7244), 74 rue Marcel Cachin, F-93017 Bobigny, France ‡ Department of Clinical Laboratory Medicine, Southwest Hospital, Third Military Medical University, 404100 Chongqing, China § Institut des Molécules et Matériaux du Mans (IMMMUMR CNRS 6283), Le Mans Université, Avenue Olivier Messiaen, 72085 Le Mans Cedex 9, France S Supporting Information *

ABSTRACT: Gold nanoparticles (GNP) are very suitable agents for thermal destruction of cancer cells because of their photothermal heating ability. In this work, photothermal properties of different sizes and shapes of GNPs were studied regarding different parameters such as GNP concentration, laser excitation intensity, and exposure time. By using the heat transfer theory, the temperature elevation in the GNP solutions was converted in temperature elevation at the GNP surface. This allows us to determine the absorption cross section (σabs) of two different sizes of spherical gold nanoparticles (GNS), which were compared with the theoretical calculations based on the Mie theory, and both results were in a good agreement. σabs was determined also for gold nanourchins with different sizes (50, 80, and 90 nm) with high precision. Finally, the temperature elevation speeds were experimentally measured for all GNPs, and we have demonstrated that they are proportional to the GNP surface area as demonstrated in the classical diffusive heat transport theory. The proposed approaches can be used to monitor the local heat generation around the GNP and pave the way to the optimization of the photothermal properties of GNPs.

1. INTRODUCTION

These optical properties due to the LSP resonance directly affect the heat generation of GNPs. A strong light absorption leads to a high heat conversion. When using a continuous wave laser, the heat is generated and dissipated into the environment continuously. Hence, the surrounding medium temperature can be increased by tens of degrees.19,20 Depending on the interaction of the GNPs with the laser, the GNP and the surrounding medium experience several possible physical phenomena, such as thermal expansion21,22 or vapor bubble formation.23−26 Because the heating efficiency depends on the LSP resonance (LSPR) position and the excitation wavelength, GNP size and shape can be tuned to increase the temperature generation by increasing the absorption cross-section of the GNP (σabs).27 Theoretically, for a spherical gold nanoparticle, the total absorption power P is described as P = σabs·I, where, I is the irradiance of the excitation laser (fixed by the experimental setup).21,28,29 While a lot of efforts were done

Recently, different types of nanovectors based on gold nanoparticles (GNPs) showed a large field of applications in cancer treatment.1−7 Owing to their unique optical and thermal properties that can be precisely tuned by changing their size, shape, or surface chemistry, they became the best candidates for cancer photothermal therapy.8,9 This thermal treatment consist of keeping the temperature of a tumor at a minimum 41 °C (temperature elevation of minimum 4 °C in the body) to cause oxidative damage because of the increment of the intracellular density of reactive oxygen species.10,11 This results in a long term cell inactivation and finally tumor cell death.12,13 The photothermal properties of GNPs directly rely on their ability to convert the absorbed light into heat. When an electromagnetic field of propagating light interacts with GNPs, it causes a collective oscillation of electrons at the surface of the nanoparticle, which is commonly called the localized surface plasmon (LSP). If the light frequency matches with the electron oscillation frequency, the GNPs present a strong absorption and scattering light.14−18 © 2019 American Chemical Society

Received: April 3, 2019 Revised: June 11, 2019 Published: June 28, 2019 17548

DOI: 10.1021/acs.jpcc.9b03122 J. Phys. Chem. C 2019, 123, 17548−17554

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The Journal of Physical Chemistry C

Figure 1. TEM images of 50GNS (a), 80GNU (b), scale bar: 20 nm. Extinction spectra of different sizes of used GNP (c).

Figure 2. Temperature elevation of the water after 15 min of excitation at different excitation power densities (0.5, 1, 2, and 3 W/cm2) in water (a), 50GNS (b), 80GNS (c), 50GNU (d), 80GNU (e), and 90GNU (f). The red line denotes the minimum temperature for the photothermal therapy.

investigate in this work how concentration, shape, and size of GNPs influence the temperature elevation in water with a new and easy experimental methodology allowing the measurement of σabs of both spherical and complex-shaped (branched) nanoparticles. Theoretical calculations based on the Mie theory and experimental measurements of the σabs of spherical (GNS) and gold nanourchins (GNU) were reported. We have demonstrated that σabs is increased by 60−80% and the temperature elevation speed in water (Ψ) is increased by 80% in the case of GNU compared to GNS. Understanding how to control the temperature elevation of branched GNPs is fundamental to manufacturing optimal nanovectors for photothermal therapy.

to understand the temperature elevation on well-defined shapes of GNPs (as spheres), especially using numerical tools, temperature elevation of the complex-shaped (branched) GNPs remains challenging.28−30 Elongated or sharp nanoparticles are much more efficient heaters than the smooth GNPs because the laser electric field is more enhanced by the hot points present at the branches, which leads to an increase of the absorption and heating properties.31−33 This makes branched gold nanoparticles the most appropriate agents for photothermal therapy.34−36 Although, the temperature elevation measurement was reported before,37−39 the main objective of our work is to propose a new and simple experimental methodology for a direct measurement of the temperature at the surface of one GNP using the heat transfer energy theory for a direct estimation of their absorption cross-section. Therefore, we 17549


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2. EXPERIMENTAL METHODS 2.1. Material. Five citrate-stabilized GNPs with different shapes (spheres −GNS− and urchins −GNU−) and diameters (50, 80, and 90 nm) were obtained from Sigma-Aldrich (ref products: 753645, 753661, 795380, 797707, 797723). The GNPs were diluted to the desired concentration (10−60 pM) in ultrapure molecular biology grade water (Gibco). 2.2. Characterization. GNP concentrations were obtained by measuring the optical extinction spectra using a UV−vis spectrometer (Kontron Instr. France) on a spectral range from 480 to 850 nm. Transmission electron microscopy (TEM) images were recorded with a JEOL JEM 1011 microscope operating (JEOL, Tokyo, Japan) as previously described by the authors.40,41 2.3. Photothermal Heating Set Up. Aqueous solutions of GNS and GNU (700 μL) with different concentrations (0, 10, 25, 50, and 60 pM) were introduced in a quartz cuvette and irradiated with an 808 nm continuous laser (Focuslight, China) at different laser irradiances (0.5, 1, 2, and 3 W/cm2) for 15 min at room temperature (23 °C or 296 K). The temperature was recorded every 30 s with a digital thermometer using a thermocouple probe (Hanna Instruments, USA) with an accuracy of 0.1 °C (see the setup in Figure S1 in the Supporting Information).

elevation with the concentration suggests that each particle is an independent heat source and there is no gradient or coupling effects, due probably to the mismatch between the LSPR and the excitation wavelength (no effect of the scattering part as reported in ref 48). Branched nanoparticles (GNUs) show a higher temperature elevation than the spherical-shaped nanoparticles (GNSs) for the same size and concentration. This is because the temperature elevation is directly related to the LSPR and the excitation wavelength. The closer is the LSPR to the laser wavelength (as in the case of GNU), the higher is the optical-thermal energy conversion as reported in refs.30,49 The linear fit of these curves shows an increase of the slope by increasing the excitation power for each type of GNP. The values of these slopes present the temperature elevation in water per picomolar of GNP ΔTw/NP (K/pM). By taking into account the solution volume (700 μL) and Avogadro number (NA), we can calculate the temperature elevation of water per nanoparticle ΔTw/NP (K/NP) using the following equation ΔTw/NP (K/NP) =

ΔTw/pM (K/pM) NA × volume

(1)

Figure 3 shows the values of temperature elevation per nanoparticle ΔTw/NP (left axis) versus different excitation

3. RESULTS AND DISCUSSION 3.1. GNP Characterization. The GNPs were characterized using TEM and UV-vis spectroscopy as shown in Figure 1. The shape and size details given by the supplier were confirmed as shown in Figure 1a,b (scale bar: 20 nm). The GNSs were mostly spherical, and the GNUs have a branched shape, as already reported by the authors in ref 42. The sizes were also confirmed by the measurement of the LSPR of the GNPs as shown in Figure 1c. The maximum LSPR wavelengths are in good agreement with the GNP shape and diameters as presented in the product technical specifications (reported is Table S1, see Supporting Information). Please note that, for photothermal therapy, the excitation wavelength should be in the near IR region. However, the majority of designed nanovectors are based on spherical and branched-shaped gold nanoparticles which have a size ranging from 10 to 60 nm (LSPR between 500 and 700 nm).8,40−43 3.2. GNP Heating Measurements under Laser Illumination. During laser heating of GNPs suspended in water, the light absorbed by the GNPs is converted into thermal energy that leads to a rise of the nanoparticle temperature. The produced heat is then transferred to the surrounding medium (water). The measurement of the different values of the temperature raise ΔT (ΔT = [T(after 15 min) − T(0)] − T(water at the same power density), with T(0) = 296 K) for different GNP concentrations (10−60 pM) excited with different laser power densities (0.5, 1, 2, and 3 W/ cm2) are shown in Figure 2. The temperature elevation of the water (without GNPs) shows a maximum of 4 K at a maximum laser power of 3 W was already demonstrated in other works,44−46 which is negligible compared to the temperature elevation in gold nanoparticle solutions (the red line denotes the minimum of temperature elevation for the photothermal therapy applications).3,47 In the case of GNPs, the temperature elevation increases linearly with the GNP concentration (linear increase of number of emitters) reaching tens of degrees. This linear dependence of the temperature

Figure 3. Temperature elevation of the water per nanoparticle ΔTw/NP (left axis) and temperature elevation of one gold nanoparticle ΔTNP (right axis) at different excitation power densities.

power densities. These curves show that the linear dependence of temperature elevation of water per nanoparticle (ΔTw/NP) with the laser irradiance. Considering the theoretical model of temperature conservation between water and gold (detailed calculations were given in the Supporting Information), the temperature elevation in water (ΔTw/NP) and the temperature at the surface of a gold nanoparticle (ΔTNP) are related by the following equation50 ΔTNP = 7.6 × 105ΔTw/NP

(2)

ij ΔTw/pM yz zz ΔTNP = 7.6 × 105jjj j NA × volume zz (3) k { The values of the temperature at the surface of a gold nanoparticle ΔTNP calculated by using eq 3 were presented in the right axis of Figure 3. Hence, we have determined

We can write, then

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Table 1. Summary of the Measured Experimental Values of α, α′, and Their Corresponding Absorption Cross-Sections Calculated Using eqs 6 and 7 R (or Req) (nm) 50GNS 80GNS 50GNU 80GNU 90GNU

experimental values of α and α′ (K·m2/W)

25 40 25 40 45

experimental absorption coefficient σabs (m2) calculated using eqs 6 and 7

−9

σabs σabs σabs σabs σabs

α = (0.38 ± 0.08) × 10 α = (1.34 ± 0.08) × 10−9 α′ = (1.80 ± 0.05) × 10−9 α′ = (3.56 ± 0.08) × 10−9 α′ = (4.08 ± 0.10) × 10−9

= = = = =

(0.71 ± 0.15) × 10−16 (4.04 ± 0.24) × 10−16 (3.39 ± 0.09) × 10−16 (10.73 ± 0.24) × 10−16 (13.84 ± 0.34) × 10−16

Figure 4. Temperature elevation in the solutions of 50 pM GNP versus time excited with 1 (a) and 2 W/cm2 (b) laser power density (dashed lines are the linear fitting of the temperature elevation curves). (c) Calculated temperature elevation speeds in water from curve fitting in (a,b) for all GNPs.

experimentally the linear dependence of the temperature at the GNP surface of different sizes and shapes with the excitation power density. Otherwise, the temperature increase in a uniform gold nanosphere with a radius R and generated by a total absorption power P was described by the theoretical models given by Baffou et al.28,29 ΔTNP

σ I P = = abs = α ·I 4πRκ w 4πRκ w

′ = ΔTNP

P 4πR eqβκ w

=

σabsI = α′·I 4πR eqβκ w

(5)

From eqs 4 and 5, we can obtain that for GNS, the absorption cross section is expressed as σabs(GNS) = α 4πRκ w

(6)

While for GNU, we can write σabs(GNU) = α′4πR eqκ w

(4)

(7)

The experimental temperature elevation values per nanoparticle (ΔTNP) at different excitation power densities shown in Figure 3 were fitted linearly by eqs 4 and 5 and the slopes α and α′ were extracted to calculate the experimental absorption cross section σabs for each type of GNP by using eqs 6 and 7 (Table 1). The experimental cross section of 50GNS is about (0.71 ± 0.15) × 10−16 m2 which is comparable to the estimated theoretical value, 0.67 × 10−16 m2, calculated by the Mie theory (see Supporting Information, Figure S2). Likewise, for 80GNS,

where σabs is the absorption cross section and I is the irradiance of the excitation light. This temperature elevation is produced by a uniformly charged sphere in a homogeneous medium (water in our case) of effective permittivity κw = 0.6 W·m−1· K−1. In the case of a nonspherical nanoparticle, a dimensionless thermal-capacitance coefficient was introduced as β, and Req is chosen as the radius of a sphere with the same volume as the particle. Hence the temperature elevation was expressed as29 17551


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The Journal of Physical Chemistry C the experimental value of σabs is about (4.04 ± 0.24) × 10−16 m2 which is very close to the theoretical value 3.54 × 10−16 m2. There results clearly validated our experimental methodology to experimentally determine σabs by measuring the temperature elevation of GNP solutions. As reported by Jiang et al.,51 the variation of the light-to-heat energy transfer efficiency of GNSs can be correlated to the absorption/extinction ratios calculated by the Mie theory for different particle sizes. The efficiency and the ratio decrease by increasing the GNS size.51 This ratio is about 0.52 for 50GNS and decreases to a value of 0.22 for 80GNS. Note that at the single particle level a larger nanoparticle would generate more heat due to its higher surface area, especially for the branched GNPs which exhibit more surface area than GNSs. By following the same methodology, we obtained in the case of GNU, the experimental values of σabs which were about (3.39 ± 0.09) × 10−16 m2 for 50GNU, (10.73 ± 0.24) × 10−16 m2 for 80GNU, and (13.84 ± 0.34) × 10−16 m2 for 90GNU. These results showed that the experimental σabs values increased with GNP size as described by the theory in eqs 6 and 7. The experimental value of σabs for 50GNU increased by a factor of 5 compared to a GNS with the same effective size (0.67 × 10−16 m2). This factor is about 3 for 80GNU and 2.5 for 90GNU. A higher value of σabs in the case of GNU compared to GNS is due to the presence of hot spots at the GNU surface and thus more light absorption. Moreover, this factor is higher for smaller GNUs which suggests that in this case the smaller GNUs are more efficient heaters because of their sharp branches. These results also demonstrate that branched nanoparticles lead to an enhancement of optical properties as already reported in refs52−55 and demonstrated by the authors.14,56 Figure 4 shows the temperature elevation ΔT(t) during 15 min in a solution of 50 pM of GNPs (corresponding to 2.1010 GNP in 700 μL of water) at 1 and 2 W/cm2 excitation power densities (ΔT(t) = T(t) − T(0), with T(0) = 296 K). For each GNP, from 0 to approximately 5 min the temperature raised linearly. Beyond 5 min, it stabilizes and reaches a maximum and constant level. The linear progression of the temperature elevation in the first few minutes (0−5 min) was fitted by a linear curve passing through the origin (dashed lines in Figure 4a,b). The slope values (Ψ) of the fitting curves were presented in Figure 4c for each type of GNP at the two excitation powers. These values represent the temperature elevation speed Ψ (K per min) for each type of GNP. We can see that for the same size (50 or 80 nm), Ψ is 80% higher for GNU than for GNS independently of the laser power. The branched shape of GNU enhances the temperature elevation speed compared to the spherical GNP. Even if the GNP sizes (effective diameters) are similar, the branched shape exhibits more contact surface with water than the spherical one, which contributes to a higher conversion of the light energy in local heat. For the same shape and by comparing the size (50GNU, 80GNU, and 90GNU), the temperature elevation speed Ψ is proportional to the effective GNP surface (GNU Ψ vs surface is presented in Figure S3 in the Supporting Information). These results are in good agreement with the theory of the classical diffusive heat transport (Fourier’s law) reported in ref 25, which describes the diffused heat by a gold nanoparticle as a function of the particle surface and the thermal conductivity.

4. CONCLUSIONS The temperature elevation of gold nanoparticles depends on many parameters such as shape, size, excitation wavelength, and power. In this work, the optical and thermal properties of different shapes and sizes of GNPs have been investigated. We have shown that the temperature elevation depends not only on the GNP LSPR position regarding the excitation wavelength but also on the GNP shape and surface. We proposed an easy experimental methodology to achieve an experimental measurement of the absorption cross section of complexshaped nanoparticles (GNU) and also spherical-shaped nanoparticles (GNS). In this latter case, the experimental values of the absorption cross-section were in a good agreement with the theoretical calculations based on the Mie theory. The results confirmed that the temperature elevation speed is also depending on GNP properties, and GNUs present enhanced thermo-optical conversion properties due to their specific shapes, inducing higher hot spots and higher surface/volume ratio. We have shown that the experimental values of the temperature elevation speed are proportional to the GNP surface as already described in the theory. This work contributes to further understanding nanoscopic photothermal effects in nanoparticles, and pave the way to the optimization of photothermal therapy for the tumor tissue treatment or drug release.

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ASSOCIATED CONTENT

S Supporting Information *

The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acs.jpcc.9b03122. Details and information about the photothermal heating set up, the gold nanoparticles technical specifications, the theoretical calculations of heat transfer between water and gold nanoparticles, the numerical calculation of extinction, absorption and scattering coefficients based on the Mie theory, and the experimental measurements of the temperature elevation speed versus gold nanoparticle surface (PDF)

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AUTHOR INFORMATION

Corresponding Author

*E-mail: [email protected]. Phone: +33 148388526. ORCID

Jolanda Spadavecchia: 0000-0001-6697-1174 Nadia Djaker: 0000-0001-7912-5436 Notes

The authors declare no competing financial interest.

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ACKNOWLEDGMENTS The authors acknowledge the ANR LOUISE project (ANR15-CE04-0001) for financial support. This work has been performed on the CNanoMat and PRISME platforms of the University Paris 13.

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Shape and Size Effect on Photothermal Heat Elevation of Gold

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