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WO2025080301A2 - Réseaux de nano-optoélectrodes nanostratifiés intégrés à une puce pour détection de tension optique non linéaire - Google Patents

Réseaux de nano-optoélectrodes nanostratifiés intégrés à une puce pour détection de tension optique non linéaire Download PDF

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Publication number
WO2025080301A2
WO2025080301A2 PCT/US2024/025411 US2024025411W WO2025080301A2 WO 2025080301 A2 WO2025080301 A2 WO 2025080301A2 US 2024025411 W US2024025411 W US 2024025411W WO 2025080301 A2 WO2025080301 A2 WO 2025080301A2
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Prior art keywords
metal
layer
insulator
conductive
gold
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WO2025080301A3 (fr
Inventor
Yuming Zhao
Chuan XIAO
Wei Zhou
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Virginia Tech Intellectual Properties Inc
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Virginia Tech Intellectual Properties Inc
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Publication of WO2025080301A2 publication Critical patent/WO2025080301A2/fr
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Anticipated expiration legal-status Critical
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65—Raman scattering
    • G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64—Fluorescence; Phosphorescence
    • G01N21/645—Specially adapted constructive features of fluorimeters
    • G01N21/648—Specially adapted constructive features of fluorimeters using evanescent coupling or surface plasmon coupling for the excitation of fluorescence
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/1717—Systems in which incident light is modified in accordance with the properties of the material investigated with a modulation of one or more physical properties of the sample during the optical investigation, e.g. electro-reflectance
    • G01N2021/1721—Electromodulation

Definitions

  • the embodiments provide a significant improvement over existing technologies and can be considered a voltage-sensitive nano-optical transducer in some cases with broad potential applications in fields such as biomolecule probes, electrophysiological optic-sensors, and opto-electro catalysis, among possibly others.
  • Aspects and advantages of embodiments of the present disclosure will be set forth in part in the following description or can be learned from the description or through practice of the embodiments. Other aspects and advantages of embodiments of the present disclosure will become better understood with reference to the appended claims and the accompanying drawings, all of which are incorporated in and constitute a part of this specification.
  • the drawings illustrate example embodiments of the present disclosure and, together with the description, serve to explain the related concepts of the present disclosure.
  • a nano-optoelectrode device includes a conductive substrate and a nano-optoelectrode coupled to the conductive substrate.
  • the nano- optoelectrode includes a metal-insulator-metal nanostructure coupled to the conductive substrate.
  • the nano-optoelectrode further includes a conductive layer coupled to the conductive substrate and to a portion of the metal-insulator-metal nanostructure.
  • the nano-optoelectrode further includes a nanocavity plasmonic hotspot formed on an exposed portion of the metal- insulator-metal nanostructure.
  • FIG.1B illustrates a top-view of an example NLNOE formed on the NLNOE array device of FIG.1A according to various aspects and embodiments of the present disclosure.
  • FIG.1C illustrates a cross-sectional side view of the NLNOE of FIG.1B according to various aspects and embodiments of the present disclosure.
  • FIGS. 2A and 2B collectively illustrate a flow diagram of an example fabrication method according to various aspects and embodiments of the present disclosure.
  • DETAILED DESCRIPTION [0012]
  • Metallic nanostructures can support surface plasmon modes and concentrate optical fields to enhance nanoscale luminescence processes ranging from spontaneous and stimulated emission, resonant and non-resonant Raman scattering, and nonlinear harmonic generation.
  • SERS surface- enhanced Raman spectroscopy
  • PES discrete plasmon-enhanced vibrational Raman scattering
  • a measured SERS spectrum often has a broad continuous emission background, typically subtracted and neglected in biochemical analyses.
  • Recent studies reveal that the SERS background can originate from plasmon- enhanced metal luminescence at hotspots.
  • the past decade has seen an increasing interest in exploring plasmon-enhanced metal luminescence for applications ranging from bioimaging to nano-thermometry and chemical reaction monitoring.
  • example NLNOEs consisting of vertically stacked and electrically connected gold-silicon dioxide-gold (Au-SiO2-Au) nanocavities can produce voltage-sensitive (up to ⁇ 30 % V -1 ) short-wavenumber ( ⁇ 93 centimeters -1 (cm) -1 ) nanoplasmonic metal luminescence signals associated with plasmon-enhanced electronic Raman scattering (PE-ERS) in physiological ionic solutions.
  • PE-ERS plasmon-enhanced electronic Raman scattering
  • a phenomenological model that can capture plasmonic, electronic, and ionic characteristics at the metal-electrolyte interface to understand several observations, including: (i) negative voltage modulation slope for PE-ERS signals, (ii) an abrupt change in PE-ERS voltage modulation slope by switching electrode voltage polarity, and (iii) reduction of PE-ERS voltage modulation slope amplitude with increasing ionic strength.
  • the model intuitively reveals that (i) the observed voltage sensitivity of PE-ERS metal luminescence signals originates from spatial overlap between the metal electronic Debye length ⁇ ⁇ ⁇ ⁇ and the 4 th power of surface plasmon field (
  • microscopic capacitive characteristics e.g., local electrolyte Debye length ⁇ ⁇ ⁇ , local dielectric permittivity ⁇ ⁇ ⁇
  • FIGS.1A to 1C illustrate different views of an example nanolaminate nano-optoelectrode (NLNOE) array device 100 according to various aspects and embodiments of the present disclosure.
  • FIG. 1A illustrates a cross-sectional side-view of the example NLNOE array device 100 according to various aspects and embodiments of the present disclosure.
  • FIGS. 1A illustrates a cross-sectional side-view of the example NLNOE array device 100 according to various aspects and embodiments of the present disclosure.
  • Each of the NLNOEs 130 in the example shown includes a multilayered metal- insulator-metal (MIM) nanostructure, nanoantenna, and nanocavity formed as a stack of alternating nanoscale MIM films deposited on the ITO layer 120 as described herein and illustrated in FIGS. 1A and 1C.
  • each of the NLNOEs 130 includes a nanolaminate nanoantenna (NLNA) 140.
  • the NLNA 140 is designed and embodied as a multilayered metal-insulator-metal (MIM) nanostructure, nanoantenna, and nanocavity.
  • the NLNA 140 is designed and embodied in this example as a gold-silicon dioxide (Au-SiO2) nanostructure, nanoantenna, and nanocavity.
  • the NLNA 140 is formed as a stack of alternating nanoscale films of gold (Au) and silicon dioxide (SiO 2 ) deposited on the ITO layer 120, although another material or materials may be relied upon in some cases.
  • a nanoscale film or films of silver (Ag) may be used in place of or in addition to such nanoscale films of gold (Au).
  • the NLNA 140 includes one or more gold (Au) films or layers 142a, 142b, 142c (or “Au layers 142”) and one or more silicon dioxide (SiO 2 ) films or layers 144a, 144b (or “SiO 2 layers 144”) deposited between the Au layers 142 as illustrated in FIGS.1A and 1C.
  • Au gold
  • SiO 2 silicon dioxide
  • the thickness of each of the Au layers 142 and the SiO2 layers 144 may be the same in some cases. In other examples, at least one of the Au layers 142 or the SiO2 layers 144 may have a thickness that is different from that of at least one other layer of the Au layers 142 or the SiO2 layers 144.
  • each of the Au layers 142 is formed to an approximate thickness of 25 nm and each of the SiO2 layers 144 is formed to an approximate thickness of 10 nm, although another thickness may be relied upon in some cases for any of the Au layers 142 or the SiO2 layers 144.
  • the NLNOEs 130 are formed on the NLNOE array device 100 according to a certain pattern. However, in some cases, the NLNOEs 130 may be formed on the NLNOE array device 100 according to a pattern that is different from that shown in FIGS. 1A and 1B.
  • the Au layer 150 can be coated on portions of a top portion or surface of the ITO layer 120 and on a top and/or side portion or surface of each NLNA 140 as illustrated in FIGS.1A to 1C.
  • the Au layer 150 is coated on portions of a top surface of the ITO layer 120, as well as on at least a portion of a top surface of each NLNA 140 (e.g., top surface of the Au layer 142c) and on at least a portion of a sidewall surface of each NLNA 140 (e.g., side surfaces of the Au layers 142 and the SiO2 layers 144).
  • an oblique- angle e-beam evaporation process can be performed to deposit the Au layer 150 on the ITO layer 120 and the NLNAs 140 at an oblique angle relative to at least one of the substrate 110 (e.g., relative to a bottom surface of the substrate 110) or the ITO layer 120 (e.g., relative to a top surface of the ITO layer 120).
  • the oblique-angle e-beam evaporation process can be performed at an oblique angle of approximately 50 degrees ( ⁇ 50°), although another angle may be relied upon in some cases.
  • depositing the Au layer 150 on portions of the ITO layer 120 and a top and/or side surface (e.g., sidewall) of each of the NLNAs 140 using the above- described oblique-angle e-beam evaporation process yields the NLNOE array device 100 having the NLNOEs 130 and metal-insulator-metal (MIM) multi-nanogap nanocavity plasmonic hotspots 160 (or “hotspots 160”). Only a single hotspot 160 is denoted in FIGS.1A to 1C for clarity.
  • MIM metal-insulator-metal
  • each hotspot 160 is formed or defined as and thus includes exposed side portions (e.g., exposed side surfaces) of the Au layers 142 and the SiO2 layers 144 where the Au layer 150 was not deposited during the oblique-angle e-beam evaporation process, due to the aforementioned tilt angle of approximately 50°.
  • the exposed side surfaces of the Au layers 142 and the SiO2 layers 144 forming each hotspot 160 are designed and fabricated such that they are not coated by the Au layer 150 and thus can be exposed to various physiological ionic solutions (e.g., electrolytes) when the NLNOE array device 100 is implemented.
  • the NLNOEs 130 are electrically and optically Attorney Docket: 222204-2870 coupled to one another, the ITO layer 120, and the substrate 110 at least in part by way of the Au layer 150.
  • the substrate 110 and the ITO layer 120 together form a conductive substrate in the example shown.
  • the substrate 110 and the ITO layer 120 together form an electrically and optically conductive substrate that is electrically and optically coupled to the NLNA 140 and the hotspot 160 of each of the NLNOEs 130 at least in part by way of the Au layer 150 as described herein and illustrated in FIGS.1A to 1C.
  • the processing steps 210, 220 collectively involve performing a reverse nanoimprinting technique to create large area, uniform NLNOE arrays on planar substrates.
  • a reusable inverse template of perfluoropolyether (PFPE) nanopillar arrays on a polyethylene terephthalate (PET) carrier substrate was replicated at the processing steps 210, 220 from a silicon master of square nanowell array (e.g., diameter ⁇ 120 nm, depth ⁇ 300 nm, and periodicity ⁇ 400 nm) by nanoimprint lithography.
  • a reverse nanoimprinting process to ultimately create a deposition mask of polymethyl methacrylate (PMMA) nanohole array patterns on planar substrates.
  • PMMA polymethyl methacrylate
  • a diluted PMMA solution can be spin-coated on a hydrophobic PFPE nanopillar array to form a PMMA layer having a nanowell array formed therein.
  • thermal nanoimprinting can then be performed at the processing step 220 to transfer the PMMA layer having the nanowell array onto an indium-tin- oxide (ITO) coated glass slide.
  • ITO indium-tin- oxide
  • the method 200 further includes releasing the PFPE template to transfer the PMMA layer 218 having the nanowell array onto the ITO layer 224 formed on the glass substrate 222.
  • the PMMA layer 218 of the PFPE template is coupled to the ITO layer 224 during the above-described thermal nanoimprinting process performed at the processing step 220.
  • the PFPE nanopillars 216 and the PET carrier substrate 212 are then released and separated from the PMMA layer 218 at the processing step 230. Upon such separation, an array of PMMA nanowells 232 are formed in the PMMA layer 218, which remains coupled to the ITO layer 224 as illustrated in FIG. 2A.
  • the method 200 further includes performing an electron- beam (e-beam) evaporation process to deposit alternating layers of gold (Au) films or layers 252 and silicon dioxide (SiO2) films or layers 254 on the PMMA layer 218 and in the PMMA nanoholes 242. Only a single layer of the Au layers 252 and a single layer of the SiO 2 layers 254 are denoted in FIG. 2B for clarity.
  • a normal-angle e-beam evaporation process can be performed at the processing step 250 to deposit alternating layers of the Au layers 252 and the SiO 2 layers 254 on the PMMA layer 218 and in the PMMA nanoholes 242 as illustrated in FIG.
  • a normal-angle e-beam evaporation process can be performed at the processing step 250 to deposit alternating layers of the Au layers 252 and the SiO 2 layers 254 on a top surface of the PMMA layer 218 and a top surface of the ITO layer 224 in the PMMA nanoholes 242 as illustrated in FIG. 2B.
  • each of the Au layers 252 is formed to an approximate thickness of 25 nm at the processing step 250 and each of the SiO2 layers 254 is formed to an approximate thickness of 10 nm, although another thickness may be relied upon in some cases for any of the Au layers 252 or the SiO2 layers 254.
  • the method 200 further includes removing the PMMA layer 218, as well as the Au layers 252 and the SiO2 layers 254 deposited on the PMMA layer 218 to yield multilayered metal-insulator-metal (MIM) nanolaminate nanoantennas (NLNA) 262 (or “NLNAs 262”) formed on the ITO layer 224. Only a single NLNA 262 is denoted in FIG. 2B for clarity.
  • MIM metal-insulator-metal
  • each of the NLNAs 262 is embodied as a gold- silicon dioxide (Au-SiO2) nanostructure, nanoantenna, and nanocavity formed as a stack of alternating nanoscale films of the Au layers 252 and the SiO2 layers 254 deposited on the ITO layer 224, although another material or materials may be relied upon in some cases.
  • Au-SiO2 gold- silicon dioxide
  • nanoantenna nanoantenna
  • nanocavity formed as a stack of alternating nanoscale films of the Au layers 252 and the SiO2 layers 254 deposited on the ITO layer 224, although another material or materials may be relied upon in some cases.
  • a nanoscale film or films of silver (Ag) may be used in place of or in addition to any or all of the Au layers 252.
  • the method 200 further includes performing an electron- beam (e-beam) evaporation process to deposit a conductive layer such as, for example, a gold (Au) layer 272 on one or more portions of the ITO layer 224 and one or more portions of the NLNAs 262.
  • a conductive layer such as, for example, a gold (Au) layer 272
  • Au gold
  • an oblique-angle e-beam evaporation process can be performed at the processing step 270 to deposit the Au layer 272 on portions of the ITO layer 224 and a top and/or side surface (e.g., sidewall) of each of the NLNAs 262 as illustrated in FIG. 2B.
  • the glass substrate 222, the ITO layer 224, and the NLNAs 262 can be tilted approximately 50°.
  • the glass substrate 222 can be positioned in a plane that is tilted approximately 50° relative to a plane that the glass substrate 222 was positioned in when the normal-angle e-beam evaporation process was performed at the processing step 250.
  • the Au layer 272 is formed to an approximate thickness of 30 nm at the processing step 270, although another thickness may be relied upon in some cases.
  • the NLNOE array device 274 illustrated in FIG.2B is an alternative example embodiment of the NLNOE array device 100 described herein with reference to FIGS. 1A to 1C.
  • the NLNOE array device 274 can include the same or similar structure, properties, and functionality as that of the NLNOE array device 100.
  • the hotspots 278 are formed on the NLNOE array device 274 as illustrated in FIG. 2B.
  • each hotspot 278 is formed or defined as and thus includes an exposed side portion or surface of a NLNA 262 where the Au layer 272 was not Attorney Docket: 222204-2870 deposited during the oblique-angle e-beam evaporation process, due to the aforementioned tilt angle of approximately 50°.
  • each hotspot 278 is formed or defined as and thus includes exposed side portions (e.g., exposed side surfaces) of the Au layers 252 and the SiO 2 layers 254 where the Au layer 272 was not deposited during the oblique-angle e-beam evaporation process, due to the aforementioned tilt angle of approximately 50°.
  • the glass substrate 222 and the ITO layer 224 together form an electrically and optically conductive substrate that can be electrically and optically coupled to one or more films, components, or structures of material formed on or otherwise coupled to such a conductive substrate as described in examples herein.
  • the glass substrate 222 and the ITO layer 224 together form an electrically and optically conductive substrate that is electrically and optically coupled to the NLNA 262 and the hotspot 278 of each of the NLNOEs 276 at least in part by way of the Au layer 272 as described herein and illustrated in FIG.2B.
  • an angled (e.g., ⁇ 50 °) deposition by e-beam evaporation can be performed to form a sidewall coating of ⁇ 30 nm thick Au on one side of NLNAs, connecting nanocavities to a conductive substrate ground to yield uniform NLNOE arrays.
  • the sidewall coating from angled e-beam deposition can enable voltage modulation of hotspots in EC-SERS measurements while leaving one side of NLNOEs uncovered to expose plasmonic nanocavity hotspots to an electrolyte environment.
  • Disjunctive language such as the phrase “at least one of X, Y, or Z,” unless specifically stated otherwise, is to be understood with the context as used in general to present that an item, term, or the like, can be either X, Y, or Z, or any combination thereof (e.g., X, Y, and/or Z).
  • Disjunctive language is not generally intended to, and should not, imply that certain embodiments require at least one of X, at least one of Y, or at least one of Z to be each present.

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  • General Health & Medical Sciences (AREA)
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Abstract

Des modes de réalisation d'un nouveau dispositif à nano-optoélectrode nanostratifié et son procédé de fabrication sont décrits. Dans un exemple, un dispositif à nano-optoélectrode comprend un substrat conducteur et une nano-optoélectrode couplée au substrat conducteur. La nano-optoélectrode comprend une nanostructure métal-isolant-métal couplée au substrat conducteur. La nano-optoélectrode comprend en outre une couche conductrice couplée au substrat conducteur et à une partie de la nanostructure métal-isolant-métal. La nano-optoélectrode comprend en outre un point chaud plasmonique à nanocavité formé sur une partie apparente de la nanostructure métal-isolant-métal.
PCT/US2024/025411 2023-04-19 2024-04-19 Réseaux de nano-optoélectrodes nanostratifiés intégrés à une puce pour détection de tension optique non linéaire Pending WO2025080301A2 (fr)

Applications Claiming Priority (2)

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US202363460556P 2023-04-19 2023-04-19
US63/460,556 2023-04-19

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WO2025080301A2 true WO2025080301A2 (fr) 2025-04-17
WO2025080301A3 WO2025080301A3 (fr) 2025-06-26

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EP2398086A1 (fr) * 2010-06-17 2011-12-21 Nederlandse Organisatie voor toegepast -natuurwetenschappelijk onderzoek TNO Dispositif opto-électrique et son procédé de fabrication
WO2014126927A1 (fr) * 2013-02-13 2014-08-21 The Board Of Trustees Of The University Of Illinois Dispositifs électroniques injectables et implantables à l'échelle cellulaire
US9983124B2 (en) * 2015-02-09 2018-05-29 Oregon State University Sensor devices comprising a metal-organic framework material and methods of making and using the same
US10274421B2 (en) * 2015-02-09 2019-04-30 Oregon State University Sensor devices comprising a metal-organic framework material and methods of making and using the same
US10695581B2 (en) * 2015-06-19 2020-06-30 The Regents Of The University Of Michigan Multicolor neural optoelectrode
WO2017139745A1 (fr) * 2016-02-13 2017-08-17 Nanoscope Technologies Llc Administration optique nano-amplifiée de molécules exogènes à des cellules et des tissus

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