Radiative Cooling of Surface-Modified Gold Nanorods upon Pulsed

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Surfaces, Interfaces, and Catalysis; Physical Properties of Nanomaterials and Materials

Radiative Cooling of Surface-Modified Gold Nanorods Upon Pulsed Infrared Photoexcitation Shao-Syuan Guo, and Li-Kang Chu J. Phys. Chem. Lett., Just Accepted Manuscript • DOI: 10.1021/acs.jpclett.8b02311 • Publication Date (Web): 21 Aug 2018 Downloaded from http://pubs.acs.org on August 22, 2018

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The Journal of Physical Chemistry Letters

Radiative cooling of surface-modified gold nanorods upon pulsed infrared photoexcitation

Shao-Syuan Guo and Li-Kang Chu*

Department of Chemistry, National Tsing Hua University, 101, Sec. 2, Kuang-Fu Rd., Hsinchu 30013, Taiwan.

Corresponding Author *To whom correspondence should be addressed. Phone: 886-3-5715131 ext. 33396. Fax: 886-35711082. E-mail: [email protected].

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ABSTRACT: Transient infrared emissions of gold nanorods capped with various materials (AuNR@X, X = CTAB, PSS, mPEG, and SiO2) upon ca. 70-s pulsed 1064-nm excitation of their longitudinal surface plasmonic bands were collected with a time-resolved step-scan Fouriertransform spectrometer. Comparing the observed emission contours with the blackbody radiation spectra revealed that parts of the additional emission intensity at low wavenumbers (13001000 cm1) were attributed to the vibrational modes of the capping materials, suggesting that the photothermal energy of AuNRs can be thermalized not only via blackbody radiation but also via radiative and non-radiative processes of the capping materials. In addition, the infrared emission of AuNR@SiO2 was more prolonged (ca. 1 ms) than those of the other three (ca. 300 µs). The photothermal energy can be efficiently randomized to the internal degrees of freedom of the soft molecular capping materials but can be stored by the rigid ones, e.g., SiO2, followed by extended radiative cooling.

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Gold nanorods (AuNRs) have been extensively utilized in photothermal therapeutic treatments, 1 photoacoustic imaging,2 and photodynamic therapeutic destruction of tumors.3 The longitudinal surface plasmonic bands of AuNRs with specific aspect ratios at the infrared region4 fit the optical therapeutic window5 for deeper light penetration. Generally, surface modification is essential for biological applications to compensate for matters of toxicity, 6 biocompatibility,6 molecular recognizability,6 and the contrast of the photoacoustic imaging systems.2 Photoexcitation of gold nanostructures leads to instantaneous heating of electrons, followed by electron-electron scattering, electron-phonon scattering and phonon-phono interaction, which increases the temperature of the surroundings. 7 Heat diffusion modelling revealed the spatial and temporal thermalization of nanoparticles with the environments on the nanoscale.8 Chen et al. demonstrated that the thermal relaxation time, τe, of a 50 nm radius gold nanosphere in water is 17.4 ns.9 Juvé et al. investigated the cooling kinetics of 426 nm noble metallic nanoparticles embedded in glass and the correlations between the interface resistance and the nanoparticle-glass acoustic mismatch.10 Hu et al. revealed that the heat dissipation from silica-coated gold nanoparticles in water is faster than that in ethanol within 100 ps. However, a dry nanoparticle film possesses a much slower thermalization time of > 300 ps.11 Additionally, the capping materials strongly affect the heat transfer from the nanorods to the environment. 12 ,13,14,15 The heat transfer of CTAB capped gold nanorods (AuNR@CTAB) to surrounding water is faster than that of gold nanorods coated with silica (AuNR@SiO2), as determined by probing the time-resolved infrared spectra of water in picoseconds.12 The thermal conductance (or conductivity) of the ligand layer on the AuNR@CTAB surface depends on the ligand concentration in solution and reaches a plateau above the ligand’s critical micelle concentration.13,14 Alternating polyelectrolyte coating layers containing poly(acrylic acid) (PAA)


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and polyallyamine hydrochloride (PAH) periodically vary the contents of apparent waters, as well as the thermal conductivity and heat capacity of the layers. 14 In addition, AuNR@SiO2 is regarded as a photoacoustic imaging nanoamplifier because its gold interfacial thermal resistance is reduced by the layer of silica.15 These aforementioned results manifest the nonradiative relaxation of the photothermal energy via phonon-phonon interactions of the AuNR and the capping materials or the solvents. However, no direct time-resolved spectroscopic observations have tracked the radiative thermalization in association with the vibrational features of the capping materials on the nanostructures, which dominate the corresponding emissive spectroscopic characteristics and kinetics. In the absence of condensed medium, photoexcited gold nanospheres in air can radiatively thermalize by emitting infrared photons, according to the blackbody radiation assumption.16 In this work, we report the transient infrared emission of dried surface-modified AuNRs with different capping materials, denoted as AuNR@X (X = CTAB, poly(styrenesulfonate) (PSS), methoxy polyethylene glycol (mPEG), and SiO2), upon 1064-nm pulsed excitation. A fundamental Nd:YAG laser operated in long pulse mode (ca. 70 s, Figure S4 in Supporting Information) was employed to excite the AuNRs to prevent severe coalescence due to the injection of much photon energy in the nanosecond domain.17 Nanosecond excitation at a peak power of 7.5 MWatt cm2 (60 mJ cm2 of an 8-ns pulse at 10 Hz repetition rate) for five minutes removed the capping materials and caused agglomeration-fusion.18 Herein, the 1064-nm fluence was controlled at 152 mJ cm2 (equivalent to a peak power of 2.2 kWatt cm2), and a step-scan Fourier-transform spectrometer was employed to record the transient infrared emission16 from the AuNR@X upon photoexcitation.


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The steady-state Vis-NIR extinction spectra of AuNRs capped with different materials are shown in Figure 1. The longitudinal surface plasmonic band of the as-prepared AuNR@CTAB peaked at 1037 nm, indicating an aspect ratio of 6.4 [Ref. 19], which agrees with the corresponding electron microscope image in Figure 2a. Because the surface of AuNR@CTAB was chemicallymodified with PSS, mPEG, and SiO2, the aspect ratios of the core AuNRs remained at 7.46.4  1.0 (Figure 2a). The slight redshift of the longitudinal bands of the AuNR@PSS, AuNR@mPEG, and AuNR@SiO2 (Figure 1) resulted from the alteration of the dielectric properties, not from the drastic change in the aspect ratios.

Figure 1. The steady-state Vis-NIR extinction spectra of AuNRs capped with various materials. AuNR@X denotes AuNRs coated with X (X = CTAB, PSS, mPEG, and SiO2). In the spectra of the neat capping materials in Figure 3, the absorbance at 2,300 cm1 can be attributed to the background CO2 which does not contribute to the emission contours. The assignments of the neat capping materials are discussed in Section 3 of the Supporting Information. The spectrum of AuNR@CTAB (Figure 3a) manifested most of the characteristics


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Figure 2. The corresponding electron microscope images of the dried AuNR@X samples (a) before and (b) after 1064-nm pulse excitation (152 mJ cm2 at 10 Hz, pulse width = ca. 70 s) for the time-resolved measurements for 80 minutes. The way to determine the aspect ratio is supplemented in the Supporting Information. of CTAB, with some residual absorbances, which might be attributed to the most intense bands of the C=C stretch mode (red fragment at ca. 1515 cm1) of the reactant hydroquinone20 and the C=O stretch mode (green fragment at ca. 1680 cm1) of the oxidation product p-benzoquinone21 in the synthesis. Some weak bands were buried at 13001000 cm1. For AuNR@PSS in Figure 3b, the bands at 2900 and 1500 cm1 could be attributed to the CTAB (marked as triangles) on the AuNR surface after wrapping by PSS, consistent with the results of Casas et al.22 and McLintock et al.23 In addition, a broad band at 16001700 cm1 could be partially attributed to the condensed water embedded in the layer of PSS. For the AuNR@mPEG in Figure 3c, most of the features of mPEG


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Relative Absorbance

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Figure 3. Infrared absorption spectra of the neat capping materials in blue and of AuNR@X (X = (a) CTAB, (b) PSS, (c) mPEG, and (d) SiO2) in black. The colored fragments are discussed in the text. The triangles marked in AuNR@PSS, AuNR@mPEG and AuNR@SiO 2 were attributed to CTAB. were observed, with a minute contribution of CTAB (marked as triangles). As for AuNR@SiO2 in Figure 3d, the main features at 12001000 cm1 were attributed to SiO2. Vibrational features at 30002800 cm1 and 1481 cm1, marked as triangles, were attributed to residual CTAB existing in the pores of the SiO2 layer, for the prepared SiO2 coating was probably partially mesoporous.24 Upon excitation with 1064 nm laser pulse, the time-resolved infrared emission contours of AuNR@X were intrinsically different (Figure 4a). The AuNR@CTAB, AuNR@PSS, and AuNR@mPEG manifested broader and quickly-decaying emission contours at 2100900 cm1. However, AuNR@ SiO2 possessed an obviously truncated infrared intensity at 1600 cm1 and prolonged emission at 12001000 cm1. The broadband emission features of these AuNR samples integrated in 100300 s (Figure 4b) partially refer to the blackbody radiation characteristics, which are spectrally structureless at 9003000 cm1 (Figure S3). However, the inconsistency of the observed and blackbody contours suggested that these extra emission features were likely to result from the capping materials. As the AuNRs absorbed the 1064 nm photons, the heat could be quickly transferred from the Au lattice to the surrounding molecules. In this work, the samples


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Figure 4. (a) Time-resolved infrared emission contours of the samples. The 1064-nm energy fluence and pulse width were 152 mJ cm2 and ca. 70 s, respectively. (b) The integrated emission contours in 100300 s (black lines) and the emission contours of the blackbody radiations at different temperatures (50200 °C). (c) The integrated emission contours in 100300 s (black lines) and steady-state infrared absorption spectra of the aforementioned samples (gray shadows). The colored fragments denote the vibrational features associated with the neat capping materials. (d) Normalized temporal profiles of the integrated infrared emission at 14001800 (red) and 10001400 (black) cm1. The gray shadow denotes the duration of the 1064 nm pulse. were prepared as dried films deposited on the CaF2 window, and the capping materials were in direct contact with the AuNR cores. As a result, the capping materials could be heated up and


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populate in their vibrationally excited states via the heating by the gold lattice and partially thermalize via the radiative processes, e.g., vibrational relaxation between the vi  vi-1 transition of the i-th vibrational mode. Interestingly, the observed extra emission intensity in 100300 s agreed with the vibrational features of the neat capping materials PSS, mPEG, and SiO2 (Figure 4c). The normalized temporal profiles of the integrated emission intensity for all AuNRs at 14001800 cm1 decayed faster than those at 10001400 cm1 (Figure 4d). This finding is consistent with the previous report that the diminishment of the infrared emission is faster at the higher wavenumber than that at the lower wavenumber during thermalization via blackbody radiation.16 In addition, AuNR@CTAB, AuNR@PSS, and AuNR@mPEG manifested quick thermalization within ca. 300 s according to the infrared emission which decayed to 10 % of the maximal intensity, whereas the decay of the infrared emission of AuNR@SiO2 was much prolonged. The softness of CTAB, PSS, and mPEG, which comprised flexible C-C skeletons, could partially benefit the quick redistribution of the internal energy via non-radiative relaxations and thermalization with the air or the substrate CaF2. In contrast, the SiO2 layer behaved like a rigid nano-blanket to prevent quick heat exchange from the AuNR to air. The infrared emission of AuNR@SiO2 concentrated at 12001000 cm1 could be ascribed to radiative relaxation through the O-Si-O phonon modes.25 The temporal profiles were consistent with a report by Nguyen et al. that the heat transfer of the photoexcited AuNR@CTAB is much faster than [email protected] In addition to the transient infrared emissions, the morphologies of the core AuNR coated with CTAB and PSS were altered after laser irradiation, as shown in Figure 2b. The AuNR@CTAB manifested severe aggregation without orientation selectivity. However, the AuNR@PSS


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exhibited end-to-end aggregations after laser irradiation. According to the observed emission contours and the blackbody emissions in Figure 4b, the temperature during the heating pulse might not have been over 200 ºC. Accordingly, photothermally-induced melting could be excluded because the sizes of these present AuNRs were not small enough for thorough melting at that temperature.

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The

CTAB

attached

to

the

AuNR

by

the

positively-charged

cetyltrimethylammonium head and formed a detergent bilayer,27,28 where the hydrophobic tails would preferentially interact with each other through van der Waals interactions.28 During infrared irradiation, the heat would destroy the van der Waals interaction and the cetyltrimethylammonium tails, exposed to air, would attract the neighboring AuNRs through hydrophobic interaction, leading to the aggregation of the AuNRs. The infrared spectrum of the AuNR@PSS sample, shown in Figure 3b, manifested the vibrational features of CTAB and PSS simultaneously, suggesting that the AuNR@PSS contained CTAB even after the purification by washing and centrifugation. This observation was consistent with a report by McLintock et al. that the added PSS will wrap the AuNR@CTAB at the surface, instead of completely replacing CTAB. In addition, the packing density of the capping CTAB at the end was less than that at the side.29,30,31 Upon photoexcitation of AuNR@PSS, the thermallyinduced destruction of aligned CTAB at the end might weaken the capping density of PSS and benefit the aggregation occurring at both ends of the AuNR@PSS, as shown in Figure 2b, leading to the orientation-selective end-to-end AuNR@PSS aggregation. In contrast, the mPEG attached to the AuNR surface via the covalent bond of Au and S, and the heat would not remove the mPEG from the surface and would rarely lead to further particle aggregation.16 Meanwhile, the rich –C2H5O moieties in mPEG also benefited the energy


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dispersion of the hot AuNR, followed by the radiative cooling at ca. 1100 cm1 and non-radiative relaxation. As expected, the AuNR@SiO2 mostly retained their core morphologies, but the coating layer of SiO2 slightly disintegrated and coalesced. We prepared the SiO2 coating using the method by Abadeer et al. [32], who demonstrated that the SiO2 layer was mesoporous. The prolonged infrared emission attributed to the O-Si-O phonon suggested that the heat could be sufficiently stored in the phonons of SiO2 and slowly released. Moreover, the CTAB caged in these pores might evaporate, thus causing these porous structures to swell or collapse. To conclude this work, we employed time-resolved infrared emission spectroscopy to record the transient thermal infrared emission upon pulsed irradiation of AuNRs coated with different capping materials. The thermal energy can be released via blackbody radiation and transferred to the capping materials. The soft capping materials (CTAB, PSS, and mPEG) are capable of quickly redistributing the heat to the vibrational degrees of freedom, mainly followed by nonradiative thermalization with minor radiative relaxation. In contrast, the SiO2 layer acts as a nano-blanket to prevent rapid heat exchange with air and mainly thermalizes via radiative cooling of the O-SiO phonon modes. These direct experimental data manifest the radiative and nonradiative relaxations selected by the capping materials on the surface-modified AuNRs. Our results provide a guide for choosing appropriate surface modifications for different thermoplasmonic applications in various time domains, such as long-term drug release or instantaneous thermotherapeutic treatments. EXPERIMENTAL METHODS


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In brief, the AuNR@CTAB were synthesized 33 and modified with PSS, 34 mPEG, 35 and SiO2.32, 36 The samples were characterized with steady-state UV-Vis absorption spectroscopy, infrared spectroscopy with a multipass attenuated total reflection37 and electron microscopy. A step-scan Fourier-transform interferometer (Vertex 80, Bruker) was employed to collect the blackbody radiation contours at different temperatures and the transient infrared emissions of the AuNR@X upon 1064 nm Nd:YAG laser excitation (Quanta Ray INDI-40-10, Spectra-Physics). The details of the experimental information are provided in the Supporting Information. ASSOCIATED CONTENT Supporting Information. Experimental setups of the step-scan Fourier-transform spectroscopy in emission mode for collecting the transient emission of AuNR (Figure S1) and blackbody emission spectra at different temperatures (Figure S2), the corresponding blackbody emission contours (Figure S3), and the temporal profile of the 1064-nm laser pulse duration (Figure S4) are supplied as Supporting Information. This material is available free of charge via the Internet at http://pubs.acs.org. AUTHOR INFORMATION To whom correspondence should be addressed. Phone: 886-3-5715131, ext. 33396. Fax: 886-35711082. E-mail: [email protected]. Notes The authors declare no competing financial interests. ACKNOWLEDGMENT


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Radiative Cooling of Surface-Modified Gold Nanorods upon Pulsed

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