Language：English   Publishing type：Research paper (scientific journal)   Publisher：Springer Science and Business Media LLC  

Abstract

Nano-objects, such as quantum dots (QDs), are essential units for the construction of functional materials and devices in current technologies. The establishment of a versatile scheme to sort desired components from a crude product is crucial for bringing out the full potential of the original materials. However, it is still challenging to separate QDs with the same composition on the basis of size and to sort QDs with the same size but different optical properties. Here, we demonstrate such sorting for the first time by combining plasmonic optical trapping with thin-layer chromatography (TLC), which is a widely used tool. LED photoexcitation of the localized surface plasmon resonance of Au nanoparticles immobilized on a TLC plate affected the distance QDs traveled depending on the wavelength and intensity of irradiated light, which led to clear separation according to the size and/or optical properties of the QDs. Since optical property-based separation cannot be achieved by conventional chromatography, in which the interactions between stationary phases of chromatographs and QDs are simply based on differences in the size or surface functionality of the QDs, the present strategy will be a key solution for the establishment of a versatile scheme for sorting nano-objects.

DOI： 10.1038/s41427-022-00414-3

Web of Science

Scopus

Other Link： https://www.nature.com/articles/s41427-022-00414-3

Authorship：Lead author   Language：English   Publishing type：Research paper (scientific journal)   Publisher：Royal Society of Chemistry (RSC)  

AuRh alloy nanoparticles, prepared by simultaneous sputter deposition of Au and Rh metals on an ionic liquid, exhibited a surface composition-dependent electrocatalytic activity.

DOI： 10.1039/d2cp01461k

Web of Science

Scopus

PubMed

Language：English   Publishing type：Research paper (scientific journal)  

We prepared a solid-state Z-scheme photocatalyst in which zinc rhodium oxide (ZnRh2O4) and bismuth vanadium oxide (Bi4V2O11) that served as hydrogen (H2) and oxygen (O2) evolution photocatalysts, respectively, were connected with gold (Au) nanoparticles. The Au nanoparticles were prepared by sputtering in an ionic liquid, N-methyl-N-propylpiperidinium bis(trifluoromethanesulfonyl)imide, to generate Au/ZnRh2O4/Au/Bi4V2O11 with various amounts of Au in the 12 mol. %-29 mol. % range (vs 1.0 mol ZnRh2O4 + 0.2 mol Bi4V2O11). Au/ZnRh2O4/Au/Bi4V2O11 photocatalyzed overall pure-water splitting under irradiation with red light at a wavelength of 700 nm, and the dependence of the amounts of Au on the apparent quantum efficiency tended to increase in the measurement range.

DOI： 10.1063/5.0010100

Web of Science

Scopus

PubMed

Authorship：Lead author   Publishing type：Research paper (scientific journal)  

Plasmon-induced charge separation (PICS) at the interface between a plasmonic nanoparticle and a semiconductor becomes less efficient as the plasmon resonance wavelength increases, because the energy of a photon may not be sufficiently higher than the interfacial Schottky barrier height. In this study, we developed PICS photocathodes by coating Au nanoparticles of different sizes on an ITO electrode with a thin TiO layer, and applied negative potentials to those photocathodes so as to suppress back electron transfer and improve the PICS photocurrent responses. The photocurrent enhancement factor was increased as the particle size was decreased, and enhancement of about two orders of magnitude was observed for small Au nanoparticles when bias voltage of 0.5 V was applied. In some cases the photocurrent enhancement was accompanied by a slight redshift of the photocurrent peak, which was caused by a lowered barrier. This technique would be useful for tuning the photocurrents when it is applied to devices such as electrochemical LSPR sensors and photodetectors. 2

DOI： 10.1039/c9pp00098d

Scopus

PubMed

Authorship：Lead author   Publishing type：Research paper (scientific journal)  

In order to improve the performance of localized surface plasmon resonance (LSPR) sensors, lattice plasmons of plasmonic nanoparticle (NP) arrays are often used. The lattice plasmon sensors based on coupling between LSPR of each NP and diffraction of the NP array generally have a higher ability to detect local refractive index changes than conventional LSPR sensors based on random NP ensembles. However, the surface selectivity of the lattice plasmon sensors is lower than that of the LSPR sensors because the local electric field of the former extends far from the particle array surface. In this work, we develop a novel plasmonic-diffractive hybrid sensor that can simultaneously determine both local and bulk refractive indices from two output signals, namely, extinction dip and peak, the wavelengths of which are differently dependent on those indices. The hybrid sensor can evaluate the refractive index changes in the immediate vicinity of the sensor surface by canceling the difference in the bulk refractive index between the sample and standard solutions.

DOI： 10.1021/acsanm.8b01829

Scopus

Authorship：Lead author   Language：English   Publishing type：Research paper (scientific journal)  

Plasmon-induced charge separation (PICS), in which an energetic electron is injected from a plasmonic nanoparticle (NP) to a semiconductor on contact, is often inhibited by a protecting agent adsorbed on the NP. We addressed this issue for an Ag nanocube-TiO system by coating it with a thin Au layer or by inserting the Au layer between the nanocubes (NCs) and TiO . Both of the electrodes exhibit much higher photocurrents due to PICS than the electrodes without the Au film or the Ag NCs. These photocurrent enhancements can be explained in terms of PICS with accelerated electron transfer, in which electron injection from the Ag NCs or Ag@Au core-shell NCs to TiO is promoted by the Au film, or PICS enhanced by a nanoantenna effect, in which the electron injection from the Au film to TiO is enhanced by optical near field generated by the Ag NC. 2 2 2 2

DOI： 10.1117/1.JPE.6.042505

Scopus

Publishing type：Research paper (scientific journal)  

Potentiometric and conductometric sensors based on localized surface plasmon resonance were developed. The sensors can be applied to coloured and turbid samples because light need not pass through the sample solution.

DOI： 10.1039/c5cc01020a

Scopus

PubMed

Authorship：Lead author   Publisher：The Electrochemical Society  

Introduction

Incident lights interact with noble metal nanoparticles (NPs) to form collective oscillations of free electrons, creating a strong electromagnetic field on their surface. This phenomenon is called localized surface plasmon resonance (LSPR). Recently metal oxide NPs with appreciable concentration of free electrons have been also reported to exhibit LSPR peaks, the peak wavelengths of which were controlled from the visible to near-IR regions.[1] When a plasmonic NP was combined with a semiconductor, the excitation of LSPR could cause the injections of electrons and/or holes from plasmonic NPs to the semiconductor, that is, the plasmon-induced charge separation (PICS).[2] Since the PICS was reported using plasmonic metal oxide NPs,[3] the intense research has been devoted to studying plasmonic metal and metal oxide NPs for the application to photovoltaics, photocatalyts, and biosensors.

Recently we reported the preparation of noble metal NPs by metal sputtering deposition onto room-temperature ionic liquids (RTIL) under a reduced pressure (RTIL/metal sputtering), where NPs of several nanometers in size were stably and uniformly dispersed without additional stabilizing agents.[4] This technique enabled the clean preparation of plasmonic metal NPs, such as Au[4], Ag[5], and AgAu alloy[6]. In this study, we apply the RTIL/metal sputtering to the preparation of molybdenum oxide (MoO_x) NPs. Thus-obtained NPs exhibited the LSPR peak, the excitation of which induced the PICS.

Experimental

The sputter deposition of molybdenum were carried out on the surface of 1-hydroxyethyl-3-methylimidazolium tetrafluoroborate (HyEMI-BF₄) and 1-ethyl-3-methylimidazolium tetrafluoroborate (EMI-BF₄) used as RTILs for 1 h with a discharge current of 30 mA under an argon pressure of 3.0 Pa. The deposited NPs were partially oxidized by the heat treatment at 473 K for 30 min in air, resulting in the formation of MoO_x NPs. The photoelectrochemical properties were measured in a 0.5 M Na₂SO₄ aqueous solution with the ITO electrode immobilized with MoO_x NPs as working electrodes, a Pt counter electrode and a Ag/AgCl reference electrode. The photocurrents were detected with monochromatic light irradiation under the potential application at +0.5 V vs Ag/AgCl.

Results and Discussion

TEM measurements revealed that Mo NPs sputter-deposited in HyEMI-BF₄ had an average diameter of 6.8 nm and then the heat treatment at 473 K increased the particle size to ca. 65 nm. XPS spectra of thus-obtained particles indicated that the thus-obtained NPs were composed of MoO_x containing Mo(V) and Mo(VI) species. The MoO_x NPs prepared in HyEMI-BF₄ showed a LSPR peak at around 840 nm, the peak wavelength of which was close to that of LSPR reported for chemically synthesized MoO_3-x NPs.[1] On the other hand, MoO_x NPs prepared in EMI-BF₄ showed no LSPR peak in the visible and near-IR regions. Anodic photocurrents were observed by the irradiation to MoO_x NP-immobilized ITO electrodes with wavelength shorter than ca. 1000 nm. Regardless of the kinds of MoO_x NPs, the action spectra of photocurrents showed the increase of IPCE at the wavelength below 600 nm due to the photoexcitation of interband transition of MoO₃, being in agreement with their extinction spectra. Furthermore, the MoO_x NPs prepared in HyEMI-BF₄ showed a peak at 840 nm, the peak wavelength of which agreed with that of their LSPR peak. In contrast, MoO_x NPs formed in EMI-BF₄ exhibited no photocurrent by the irradiation of near-IR lights.

Conclusively, we successfully prepared the MoO_x NPs with RTIL/metal sputtering technique followed by the heating treatment. The NPs formed in HyEMI-BF₄ showed the LSPR peak in near-IR region, the photoexcitation of which induced the PICS from the MoO_x NPs to the ITO electrodes.

References

(1) A. Agrawal, S. H. Cho, O. Zandi, S. Ghosh, R. W. Johns, and D. J. Milliron, Chem. Rev., 118, 3121 (2018).

(2) Y. Tian and T. Tatsuma, J. Am. Chem. Soc., 127, 7632 (2005).

(3) S. H. Lee, H. Nishi, and T. Tatsuma, Nanoscale, 10, 2841 (2018).

(4) T. Torimoto, K. Okazaki, T. Kiyama, K. Hirahara, N. Tanaka, and S. Kuwabata, Appl. Phys. Lett., 89, 243117 (2006).

(5) T. Suzuki, K. Okazaki, T. Kiyama, S. Kuwabata, and T. Torimoto, Electrochemistry, 77, 636 (2009).

(6) K. Okazaki, T. Kiyama, K. Hirahara, N. Tanaka, S. Kuwabata, and T. Torimoto, Chem. Commun., 6, 691 (2008).

DOI： 10.1149/ma2020-02592962mtgabs

Other Link： https://iopscience.iop.org/article/10.1149/MA2020-02592962mtgabs/pdf

Publisher：The Electrochemical Society  

Since the Fujishima effect was reported in 1972 [1], researches on photocatalytic water splitting using sunlight have been progressing as a method for producing hydrogen (H₂), which attracts attention as an alternative clean energy source for fossil fuels. For the effective use of sunlight, we have investigated an all-solid-state Z-scheme photocatalyst that can be sensitive to long-wavelength, low-energy light and can decompose pure water (without chemicals as a sacrificial agent or pH adjuster). In our previous study, we fabricated the Z-scheme photocatalyst, consisting of zinc rhodium oxide (ZnRh₂O₄) and bismuth vanadium oxide (Bi₄V₂O₁₁) as a H₂- and oxygen (O₂)-evolution photocatalyst, respectively, and gold (Au) as a solid redox mediator (ZnRh₂O₄/Au/Bi₄V₂O₁₁). The photocatalyst has successfully achieved the overall pure water splitting irradiated with red light (wavelength 700 nm) via Au, which mediated the transfer of photoexcited electrons from the conduction band (CB) of Bi₄V₂O₁₁ to the valence band (VB) of ZnRh₂O₄. Then, photogenerated holes in the VB of Bi₄V₂O₁₁ and photoexcited electrons in the CB of ZnRh₂O₄ effectively oxidized and reduced water, respectively, to achieve overall water splitting [2].

One of the co-authors (T.T.) reported a simple technique using a sputtering method to synthesize Au nanoparticles (Au_sp), much smaller than commercially available Au [3]. In the synthesis procedures described below, some part of Au_sp, supported only on the surface of ZnRh₂O₄, functions as a co-catalyst for H₂ evolution. Thus, it was expected that Au_sp could be homogeneously distributed as the redox mediator and co-catalyst, resulting in the improvement of the water splitting reaction. In this study, various concentrations of Au_sp in ZnRh₂O₄/Au_sp/Bi₄V₂O₁₁ were prepared, and the dependence of Au_sp concentration on water-splitting activity was evaluated.

Au_sp were evenly deposited by sputtering onto an ionic liquid (PP13-TFSI; N-methyl-N-propylpiperidinium bis(trifluoromethanesulfonyl)imide). Before performing the process, treatments of heating and stirring were performed in a vacuum atmosphere so as to extract air and water from the ionic liquid. ZnRh₂O₄ and Bi₄V₂O₁₁ powders were prepared by a solid-state reaction method. ZnO and Rh₂O₃ powders, and Bi₂O₃ and V₂O₅ powders as starting materials were uniformly mixed in a stoichiometric ratio to prepare ZnRh₂O₄ and Bi₄V₂O₁₁, respectively. The mixture was pelletized and calcined at 1150 °C for ZnRh₂O₄ for 24 h and 850 °C for Bi₄V₂O₁₁ for 8 h, then pulverized to obtain ZnRh₂O₄ and Bi₄V₂O₁₁ powders. ZnRh₂O₄ were added to the prepared Au_sp containing in PP13-TFSI and the mixture was heated and stirred in a nitrogen atmosphere in a test tube for 280 °C for 1 h (the expected molar percentage of Au to ZnRh₂O₄ was 2, 10, 12, and 17 mol%). Next, PP13-TFSI was removed by centrifugation and drying overnight to produce ZnRh₂O₄+Au_sp. ZnRh₂O₄/Au_sp was obtained by calcining the ZnRh₂O₄+Au_sp at 850 ° C for 2 h to strengthen the connection. ZnRh₂O₄/Au_sp/Bi₄V₂O₁₁ was produced by mixing Bi₄V₂O₁₁with ZnRh₂O₄/Au_sp at a ratio of 20 mol% with respect to ZnRh₂O₄ and following the same procedure as for producing Bi₄V₂O₁₁.

As-prepared Au_sp size distribution was determined by measuring the size of individual particles in the TEM image, and the average particle size was 2.3 nm. The average particle size of Au_sp containing in ZnRh₂O₄+Au_sp, ZnRh₂O₄/Au_sp and ZnRh₂O₄/Au_sp/Bi₄V₂O₁₁ after heat treatment was 9.0 nm, 27 nm, and 42 nm. Thus, it was confirmed that Au_sp could be used in the Z-scheme photocatalyst with the particle size much smaller than that of the commercial Au (300-500 nm) [2]. The amount of Au containing in ZnRh₂O₄/Au_sp/Bi₄V₂O₁₁ was estimated from XPS. Since Au_sp is mainly bonded to the surface of ZnRh₂O₄, we estimated the Au_sp amount based on the Bi 4f peak of Bi₄V₂O₁₁, which is unlikely to be affected by the change of Au_sp amount when measured by XPS. Then, the estimated Au_sp amounts were 12, 18, 20, and 29 mol% (vs. 1.0 mol of ZnRh₂O₄ + 0.2 mol of Bi₄V₂O₁₁). All photocatalysts were confirmed that H₂and O₂ were generated from pure water at a ratio of approximately 2 : 1 by irradiation of red light with a wavelength of 700 nm. The water splitting activity tended to be proportional to the amount of Au_sp estimated from XPS. These will be discussed in detail at the conference.

[1] A. Fujishima and K. Honda, Nature, 238, 37 (1972)

[2] K. Kamijyo, T. Takashima, M. Yoda, J. Osaki, and H. Irie, Chem. Commun., 54, 7999 (2018)

[3] T. Torimoto, K. Okazaki, T. Kiyama, K. Hirahara, N. Tanaka, and S. Kuwabata, Appl. Phys. Lett., 89, 243117 (2006)

DOI： 10.1149/ma2020-02613118mtgabs

Other Link： https://iopscience.iop.org/article/10.1149/MA2020-02613118mtgabs/pdf

Authorship：Lead author  

Publisher：The Electrochemical Society  

Introduction

Light incident on metal thin films or nanoparticles (NPs) may induce a collective oscillation of conduction electrons that can lead to generation of strong electromagnetic fields in the vicinity of the metal surfaces. This phenomenon is commonly referred to as surface plasmon resonance (SPR) for metal films and localized surface plasmon resonance (LSPR) for metal NPs. These plasmon resonances have been applied to affinity-based sensing due to their sharp response to refractive index changes in the vicinity of the metal surface. Although LSPR sensors can be smaller and less expensive than SPR sensors, they are not suitable for colored or turbid sample solutions in general because light must pass through the sample to an optical detector. In this study, LSPR sensors that directly output potential changes were developed (Figure 1).¹ The sensors are based on plasmon-induced charge separation (PICS),²in which excited conduction electrons in metal NPs transfer to the semiconductor in direct contact with the NPs. Since light need not pass through the sample solution, the sensor can be applied to colored and turbid sample liquids.

Experimental

TiO₂ thin films (~70 nm thick) were prepared on ITO-coated glass plates by a spray pyrolysis method from 2-propanol containing titanium diisopropoxide bis(acetylacetonate) followed by annealing at 500 °C for 30 min. Citrate-protected Au NPs (40 nm) were adsorbed onto the TiO₂ surface by immersing the substrate in a Au NP dispersion at pH 2.7 for 6 h. Au@TiO₂ core-shell NPs were also used instead of Au NPs. The Au NPs were covered with 5–7 nm-thick TiO₂shells.

The open-circuit potential (OCP) measurements were conducted with the Au NP/TiO₂/ITO working electrode in water (refractive index n = 1.33) and a Ag|AgCl reference electrode. The working electrode was irradiated with light of different wavelengths, and a negative potential shift upon the light irradiation was measured. Refractive index of the solution was changed by adding glycerol (n= 1.47) to water and peak shifts in the photopotential action spectra were detected.

Results and Discussion

a) Sensors with Au NPs. The Au NP/TiO₂/ITO electrode was irradiated with light and a negative shift of the OCP was observed. The photoresponse is ascribed to injection of electrons from resonant Au NPs to the conduction band of TiO₂ due to PICS. In Figure 2, typical potential shifts –ΔE at t = 60 s (light irradiation was started at t = 0 s) are plotted against the energy of irradiated photons. The photopotential action spectrum is in good agreement with the LSPR absorption spectrum in shape. Furthermore, the peak in the action spectrum was redshifted in response to an increase in the refractive index of the sample solution. This peak wavelength shift was plotted against the refractive index of solutions, and a linear relationship was obtained. The refractive index sensitivity was calculated to be 33 ± 4 nm RIU^-1 (refractive index unit). The sensor was applied to coffee as a colored and turbid sample. The Au/TiO₂film in coffee did not show any extinction peak but a clear photopotential peak.

b) Sensors with Au@TiO₂ NPs. Since the refractive index sensitivity was not sufficiently high, we replaced the Au NPs with Au@TiO₂ NPs. As a result, the sensitivity was increased to 72 nm RIU^-1. In the case of the bare Au NPs, electron oscillation is somewhat localized at the bottom of each NP, at which the NP is in contact with TiO₂, so that certain volume of the sensing region is occupied by the TiO₂ substrate. On the other hand, the electron oscillation is delocalized over the whole NP surface for the Au@TiO₂ NPs because the Au core is fully covered with the TiO₂ shell, and therefore the masking by the TiO₂substrate is less significant.

Conclusion and Future Plan

The LSPR sensor which directly output electrical signals from TiO₂loaded with Au NPs was developed. The photopotential peaks were obtained on the basis of PICS. The response peak redshifted linearly as the refractive index of the sample solution increased. Since light need not pass through a sample solution, the sensor can be applied to a colored and turbid sample liquid. Work is currently underway to improve the sensor performance by using anisotropic NPs.

References

(1) T. Tatsuma, Y. Katagi, S. Watanabe, K. Akiyoshi, T. Kawawaki, H. Nishi, and E. Kazuma, Chem. Commun., 51, 6100 (2015).

(2) Y. Tian and T. Tatsuma, J. Am. Chem. Soc., 127, 7632 (2005).

Figure Caption. (a) Mechanism of the potentiometric LSPR sensor. (b) Typical photopotential action spectra of a Au/TiO₂ film.

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Figure 1

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DOI： 10.1149/ma2016-02/53/3919

Other Link： https://iopscience.iop.org/article/10.1149/MA2016-02/53/3919/pdf

Authorship：Lead author   Language：Japanese   Publisher：電気化学会化学センサ研究会  

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