WO2024254473A1 - Verre émettant des ultraviolets et son procédé de fabrication - Google Patents

Verre émettant des ultraviolets et son procédé de fabrication Download PDF

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Publication number
WO2024254473A1
WO2024254473A1 PCT/US2024/033043 US2024033043W WO2024254473A1 WO 2024254473 A1 WO2024254473 A1 WO 2024254473A1 US 2024033043 W US2024033043 W US 2024033043W WO 2024254473 A1 WO2024254473 A1 WO 2024254473A1
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WIPO (PCT)
Prior art keywords
light
article
emitting layer
biofouling
substrate
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Ceased
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PCT/US2024/033043
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English (en)
Inventor
Mariana LANZARINI-LOPES
Katrina FITZPATRICK
Leila Alidokht AKHOONI
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University of Massachusetts Amherst
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University of Massachusetts Amherst
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Priority to EP24820144.4A priority Critical patent/EP4724406A1/fr
Publication of WO2024254473A1 publication Critical patent/WO2024254473A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
    • C03C17/007—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character containing a dispersed phase, e.g. particles, fibres or flakes, in a continuous phase
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
    • C03C17/008—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character comprising a mixture of materials covered by two or more of the groups C03C17/02, C03C17/06, C03C17/22 and C03C17/28
    • C03C17/009—Mixtures of organic and inorganic materials, e.g. ormosils and ormocers
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/40—Coatings comprising at least one inhomogeneous layer
    • C03C2217/42—Coatings comprising at least one inhomogeneous layer consisting of particles only
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/40—Coatings comprising at least one inhomogeneous layer
    • C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
    • C03C2217/44—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the composition of the continuous phase
    • C03C2217/445—Organic continuous phases
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/40—Coatings comprising at least one inhomogeneous layer
    • C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
    • C03C2217/46—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase
    • C03C2217/48—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase having a specific function

Definitions

  • the present patent document is directed generally to devices configured to provide a UV-light emission having disinfecting properties. Methods of making and using the same are also disclosed.
  • BACKGROUND [004] Biofouling on the exterior surface of marine vessels and equipment creates significant operational, functional, and financial hurdles.
  • a biofilm refers to a structured collection of microorganisms that adhere to surfaces through the production of extracellular polymeric substances (EPS).
  • EPS extracellular polymeric substances
  • Early-stage biofilm begins to form during initial vessel submersion, developing slime and growing into complex biofouling communities of barnacles, sponges, and tunicates within days. Biological growth and the bio-corrosion associated with biofilms can damage oceanographic equipment and decrease the optical transparency of windows used for cameras and communications devices.
  • Biocidal coatings employ an active agent to kill fouling organisms.
  • Non-biocidal coatings include silicone- based fouling release coatings and those designed to be mechanically resistant to abrasive cleaning.
  • UVC ultraviolet light between 250 and 280 nm wavelengths
  • an article comprising (a) a light-emitting layer; and (b) one or more UV light sources coupled within the article such that a Attorney Docket No.11555-010WO1 UMA2023-053-01 light beam is side-emitted by the light-emitting layer in a direction substantially perpendicular to a direction of the light beam; wherein the light-emitting layer comprises a plurality of light-scattering elements and exhibits at least 90% transmittance.
  • a method of comprising: forming an article by coupling one or more UV light sources such that a light beam is side-emitted by a light-emitting layer in a direction substantially perpendicular to the direction of the light beam; wherein the light-emitting layer comprises a plurality of light-scattering elements and exhibits at least 90% transmittance; wherein the article is at least partially disinfecting and/or anti-biofouling.
  • Also disclosed is a method comprising: forming any of the disclosed herein articles; exposing the article to a biofouling environment such that the light- emitting layer at least partially faces the biofouling environment, passing a light beam from the one or more UV-light sources to initiate a side-emission of the UV light, and reducing biofouling at at least a portion of a surface of the article that is exposed to the biofouling environment.
  • FIGURE 1A is a perspective view of an embodiment of a biofouling- resistant device made in accordance with the present disclosure.
  • FIGURE 1B is a perspective view of a vessel, including an embodiment of a biofouling-resistant device made in accordance with the present disclosure.
  • FIGURE 2 shows a plan view of an exemplary embodiment of an experimental setup of a biofouling-resistant device made in accordance with the present disclosure.
  • FIGURE 3A shows a chart of UV irradiance measurements for slides coated with different concentrations of nanoparticles with a transparent polymer coating, where dilution values of 1 to 0, 1 to 2, 1 to 5, 1 to 10, 1 to 100, and 0 to 1 represent the slides coated with 265, 132.5, 53, 26.5, 2.65, and 0 ⁇ g/cm 2 of nanoparticles, respectively.
  • FIGURE 3B shows a chart of UV irradiance measurements for slides coated with different concentrations of nanoparticles without a transparent polymer coating, where dilution values of 1 to 0, 1 to 2, 1 to 5, 1 to 10, 1 to 100, and 0 to 1 represent the slides coated with 265, 132.5, 53, 26.5, 2.65, and 0 ⁇ g/cm 2 of nanoparticles, respectively.
  • FIGURE 4A shows a chart of transparency of slides coated with different concentrations of nanoparticles without a transparent polymer coating, where dilution values of 1 to 0, 1 to 2, 1 to 5, 1 to 10, 1 to 100, and 0 to 1 represent the slides coated with 265, 132.5, 53, 26.5, 2.65, and 0 ⁇ g/cm 2 of nanoparticles, respectively.
  • FIGURE 4B shows a chart of transparency of slides coated with different concentrations of nanoparticles with a transparent polymer coating, where dilution values of 1 to 0, 1 to 2, 1 to 5, 1 to 10, 1 to 100, and 0 to 1 represent the slides coated with 265, 132.5, 53, 26.5, 2.65, and 0 ⁇ g/cm 2 of nanoparticles, respectively;
  • FIGURE 5 is a chart of the final UV emission profile and the UV spectrum (inset) for the experimental setup used in the submersion shown in FIG.2. The decrease in irradiance is due to the presence of a sealing polymer.
  • FIGURE 6A shows a photograph of control glasses after immersion for 20 days, showing relative abundance and biofilm coverage thereon.
  • FIGURE 6B shows a photograph of biofouling-resistant devices made in accordance with the present disclosure after immersion for 20 days, showing relative abundance and biofilm coverage thereon.
  • Attorney Docket No.11555-010WO1 UMA2023-053-01 [024]
  • FIGURE 6C shows a graph comparing the average values of the experimental results shown in FIGS.6A-6B.
  • FIGURE 7A shows a graph of the average number of CFU/cm 2 of cells of the experimental results.
  • FIGURE 7B shows a graph of the average number of live cells/ cm 2 of the experimental results.
  • FIGURE 7C shows a graph of the average number of dead cells/ cm 2 of the experimental results.
  • FIGURE 8 shows a graph of the concentration of total DNA, unbound, and bound protein in the experimental results.
  • FIGURE 9 shows a schematic of each layer of an exemplary article according to one aspect.
  • FIGURES 10A-10C show photographs of exemplary articles with and without polymer coatings.
  • FIG.10A shows an exemplary planar glass substrate coated with a light-emitting layer comprising a plurality of nanoparticles and a layer of a UV-transparent polymer.
  • FIG.10B shows a lens as a glass substrate coated with a light-emitting layer comprising a plurality of nanoparticles and a layer of a UV-transparent polymer.
  • FIG.10C shows a control glass lens without coating to show optical transparency.
  • FIGURE 11 shows the UV measurement setup for a 100 mm (diameter) x 6 mm (thickness) lens.
  • FIGURE 12 shows an example case design for the submersion of UV side-emitting glass (UEGs) in a marine environment.
  • FIGURES 13A-13F show the UV emission profiles of UEG at 275 nm.
  • FIGURES 14A-14C show the UV emission profiles of UEG at 265 nm.
  • FIGURES 15A-15B show AFM top view images of a glass surface coated with only polymer (a1) and nanoparticles + polymer (b1).
  • FIGURES 16A-16B show corresponding cross-sectional profiles (a2 and b2) of the AFM images shown in FIGs.15A-15B.
  • Attorney Docket No.11555-010WO1 UMA2023-053-01 [037]
  • FIGURES 17A-17B demonstrate that silicone sealing decreases UV irradiance from an exemplary article.
  • FIGURE 18 shows that the materials with high absorption coefficients have high refractive indices.
  • FIGURE 20 demonstrates that the PTFE coating omitted the adverse effect of silicon on UV irradiance
  • FIGURES 21A-21C show the experimental setup for the use of an exemplary article.
  • FIGURE 22 shows a significant inhibitory effect (92%) of UEGs on the biofilm growth based on visual assessment.
  • FIGURE 23 shows a decrease in live cell count in biofilm coverage based on CFU.
  • FIGURE 24 shows an exemplary setup of an exemplary article in one aspect of the disclosure.
  • FIGURE 25 shows the UV emission profiles of UEG slides at multiple wavelengths. The slides used as a substrate were 24 mm (W) x 110 mm (L) x 2 mm (T).
  • FIGURE 26 shows the results of UEGs submerged with Pseudomonas bacteria.
  • FIGURE 27 shows the results of UEGs submerged with mixed marine bacteria.
  • FIGURE 28 shows electrical power per order.
  • FIGURE 29 shows optical coherence tomography (OCT) images of biofilm.
  • OCT optical coherence tomography
  • FIGURE 30 shows measuring biofilm thickness at the areas covered by biofilm.
  • FIGURE 31 compares the effectiveness of UEG with external UV irradiation.
  • an amount, size, formulation, parameter, or other quantity or characteristic is “about,” “approximate,” or “at or about,” whether or not expressly stated to be such. Where "about,” “approximate,” or “at or about” is used before a quantitative value, the parameter also includes the specific quantitative value itself unless expressly stated otherwise.
  • the term or phrase “effective,” “effective amount,” or “conditions effective to” refers to such amount or condition that is capable of performing the function or property for which an effective amount or condition is expressed. As will be pointed out below, the exact amount or particular condition required will vary from one aspect to another, depending on recognized variables such as the materials employed and the processing conditions observed.
  • the range can also be expressed as an upper limit, e.g., 'x, y, z, or less' and should be interpreted to include the specific ranges of ‘x,’ ‘y,’ ‘z,’ 'about x,' 'about y,' and 'about z' as well as the ranges of 'less than x,' 'less than y, or 'less than z,' or 'less than about x,' 'less than about y, and 'less than about z.' Likewise, the phrase ' x, y, z, or greater' should be interpreted to include the specific ranges of ‘x,’ ‘y,’ ‘z,’ 'about x,' 'about y,' and 'about z' as well as the ranges of 'greater than x,' greater than y,' 'greater than z,' or 'greater than about x,' greater than about y,' 'greater than about z
  • a numerical range of " 0.1% to 5%” should be interpreted to include not only the explicitly recited values of 0.1% to 5% but also include individual values (e.g., 1%, 2%, 3%, and 4%) and the sub-ranges (e.g., 0.5% to 1.1%; 0.5% to 2.4%; 0.5% to 3.2%, and 0.5% to 4.4%, and other possible sub-ranges) within the indicated range.
  • Recitation of ranges of values herein is merely intended to serve as a shorthand method of referring individually to each separate value recited or falling within the range unless otherwise indicated herein, and each separate value is incorporated into the specification as if it were individually recited.
  • Ranges provided herein are understood to be shorthand for all of the values within the range.
  • a range of 1 to 50 is understood to include any number, or combination of numbers, from the group consisting of 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, or 50 or sub-ranges from the group consisting of 10-40, 20-50, 5-35, etc.
  • composition is intended to encompass a product comprising the specified ingredients in the specified amounts, as well as any product that results, directly or indirectly, from a combination of the specified ingredients in the specified amounts.
  • references in the specification and concluding claims to parts by weight of a particular element or component in a composition denote the weight relationship between the element or component and any other elements or components in the composition or article for which a part by weight is expressed.
  • components Y, X, and Y are present at a weight ratio of 2:5 and are present in such a ratio regardless of whether additional components are contained in the mixture.
  • Attorney Docket No.11555-010WO1 UMA2023-053-01 [069] A weight percent (wt.%) of a component, unless specifically stated to the contrary, is based on the total weight of the formulation or composition in which the component is included.
  • the term “substantially” can, in some aspects, refer to at least about 80 %, at least about 85 %, at least about 90 %, at least about 91 %, at least about 92 %, at least about 93 %, at least about 94 %, at least about 95 %, at least about 96 %, at least about 97 %, at least about 98 %, at least about 99 %, or about 100 % of the stated property, component, composition, or other condition for which substantially is used to characterize or otherwise quantify an amount.
  • the term “substantially free,” when used in the context of a composition or component of a composition that is substantially absent, is intended to refer to an amount that is then about 1 % by weight, e.g., less than about 0.5 % by weight, less than about 0.1 % by weight, less than about 0.05 % by weight, or less than about 0.01 % by weight of the stated material, based on the total weight of the composition or based on any other calculations as disclosed.
  • the term “substantially,” in, for example, the context “substantially identical” or “substantially similar,” refers to a method or a system, or a component that is at least about 90%, at least about 91%, at least about 92%, at least about 93%, at least about 94%, at least about 95%, at least about 96%, at least about 97%, at least about 98%, at least about 99%, or about 100% by similar to the method, system, or the component it is compared to.
  • the terms “substantially identical reference composition” and “substantially identical reference article” refer to a reference composition or article comprising substantially identical components in the absence of an inventive component.
  • the term “substantially,” in, for example, the context “substantially identical reference composition” or “substantially identical reference article,” refers to a reference composition or an article comprising substantially identical components and wherein an inventive component is absent or is substituted with a common in the art component.
  • contact or other forms of the word, such as “contacted” or “contacting,” it is meant to add, combine, or mix two or more compounds, compositions, or materials under appropriate conditions to produce a desired product or effect.
  • react is sometimes used when “contacting” results in a chemical reaction.
  • Spatially relative terms such as,“ “beneath,” “below,” “lower,” “above,” “upper,” “upward,” “downward,” “top,” “bottom,” and the like, can be used herein for ease of description to describe one element or feature's relationship to another element(s) or feature(s) as illustrated in the figures.
  • the spatially relative terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures. For example, if the device in the figures is turned over, elements described as “below” or “beneath” other elements or features would then be oriented “above” the other elements or features. Thus, the term “below” can encompass both an orientation of above and below.
  • the device can be otherwise oriented (rotated 90 degrees or at other orientations), and the spatially relative descriptors used herein are interpreted accordingly.
  • a “UV-transparent material” refers to a material that, in a selected wavelength range, typically has an average percent transmission of least 80%, at least 85%, at least 90%, or at least 95 % over the desired wavelength range.
  • a material that is substantially UV-C transparent typically has an average percent transmission of at least 80%, at least 85%, and at least 90 % over the UV-C wavelength range.
  • the term “light-emitting layer” refers to a light-side- emitting layer, a light-face-emitting layer, or a combination thereof.
  • Disclosed herein are materials, compounds, compositions, and components that can be used for, can be used in conjunction with, can be used in preparation for, or are products of the disclosed methods and compositions. These and other materials are disclosed herein, and it is understood that when combinations, subsets, interactions, groups, etc., of these materials, are disclosed while specific reference of each various individual and collective combinations and permutation of these compounds may not be explicitly disclosed, each is specifically contemplated and described herein.
  • compositions are disclosed and a number of modifications that can be made to a number of components of the composition are discussed, each and every combination and permutation that is possible are specifically contemplated unless specifically indicated to the contrary.
  • a class of components A, B, and C are disclosed and a class of components D, E, and F and an example of a combination composition A-D are disclosed, then even if each is not individually recited, each is individually and collectively contemplated.
  • each of the combinations A-E, A-F, B-D, B-E, B-F, C-D, C-E, and C-F are specifically contemplated and should be considered disclosed from the disclosure of A, B, and C; D, E, and F; and the example combination A-D.
  • any subset or combination of these is also specifically contemplated and disclosed.
  • the sub-group of A-E, B-F, and C-E are specifically contemplated and Attorney Docket No.11555-010WO1 UMA2023-053-01 should be considered disclosed from disclosure of A, B, and C; D, E, and F; and the example combination A-D.
  • an article comprising (a) a light-emitting layer; and (b) one or more UV light sources coupled within the article such that a light beam is side-emitted by the light-emitting layer in a direction substantially perpendicular to a direction of the light beam; wherein the light-emitting layer comprises a plurality of light-scattering elements and exhibits at least 90% transmittance.
  • the light-emitting layer can exhibit at least 91% transmittance, at least 92% transmittance, at least 93% transmittance, at least 94% transmittance, at least 95% transmittance, at least 96% transmittance, at least Attorney Docket No.11555-010WO1 UMA2023-053-01 97% transmittance, at least 98% transmittance, at least 99% transmittance, at least 99.5% transmittance, or at least 99.9 % transmittance.
  • the light-emitting layer can exhibit transmittance in a range of 90% to 100%, including 90%-99%, 90%-98%, 90%-98%, 90%-97%, 90%-96%, 90%-95%, 90%-95%, 90%- 93%, 90%-92%, 91%-100%, 92%-100%, 93%-100%, 94%-100%, 95%-100%, 96%-100%, 97%-100%, 98%-100%, and so on.
  • the light-emitting layer can be used as a separate layer.
  • the light-emitting layer can be positioned on a substrate.
  • the substrate can be transparent or non-transparent.
  • the light-emitting layer can be at least partially embedded within the substrate.
  • the light-emitting layer when the substrate is transparent, can be at least partially embedded within the bulk of the substrate adjacent to at least one surface of the substrate.
  • the light-emitting layer can be formed during the formation of the substrate itself, or it can be embedded into a formed substrate by any method known in the art.
  • the plurality of light-scattering elements comprise a plurality of particles.
  • the plurality of particles is a plurality of nanoparticles.
  • the plurality of nanoparticles can have any size to achieve the desired light emission.
  • the nanoparticles can have a size of 50 nm to 500 nm, including exemplary values of 80 nm, 100 nm, 120 nm, 150 nm, 180 nm, 200 nm, 220 nm, 250 nm, 280 nm, 300 nm, 320 nm, 350 nm, 380 nm, 400 nm, 420 nm, 450 nm, and 480 nm. It is understood that the plurality of nanoparticles can have any size that falls between any two foregoing values or falls within a range formed by any two foregoing values.
  • the size of the nanoparticles can be 50 nm to 450 nm, 50 nm to 400 nm, 50 nm to 350 nm, 50 nm to 300 nm, 50 nm to 250 nm, 50 nm to 200 nm, 50 nm to 150 nm, 50 nm to 100 nm, 100 nm to 500 nm, 150 nm to 500 nm, 200 nm to 500 nm, 250 nm to 500 nm, 300 nm to 500 nm, 350 nm to 500 nm, 400 nm to 500 nm, or 450 nm to 500 nm and so on.
  • the size of the light-scattering elements can be chosen at least in part upon the light wavelength being employed to achieve the desired scattering of the UV light.
  • the desired size of the light-scattering elements is Attorney Docket No.11555-010WO1 UMA2023-053-01 chosen to provide substantially equal and uniform scattering at all wavelengths in the desired range (which is disclosed below).
  • the size of the light-scattering elements can be chosen such that the scattering is not uniform at all the wavelengths. [088] It is understood that any nanoparticles that can provide the desired effect can be used.
  • the nanoparticles can comprise silica.
  • the plurality of nanoparticles can comprise glass, metal oxides, zeolites, polymer particles (for example, PMMA, PVC, acrylates, and so on), or any combination thereof.
  • the nanoparticles can be functionalized or unfunctionalized.
  • silica nanoparticles can be functionalized with amine groups forming aminated silica nanoparticles.
  • the aminated silica nanoparticles can exhibit a positive charge.
  • the nanoparticles when the nanoparticles have at least a partial charge, the nanoparticles can be disposed on any substrate using electrostatic deposition.
  • silica beads of any of the disclosed sizes can be used as a light-scattering element.
  • the plurality of light-scattering elements can comprise one or more of a plurality of particles (or nanoparticles), defects, air bubbles, or a combination thereof. Any of the disclosed above plurality nanoparticles can be used herein. It is understood that other defects and air bubbles can also be formed during glass (when used as a transparent substrate, for example) manufacturing.
  • the light-emitting layer can have a thickness of 50 nm to 5 cm, including exemplary values of 100 nm, 250 nm, 500 nm, 750 nm, 1 micron, 25 microns, 50 microns, 100 microns, 250 microns, 500 microns, 750 microns, 1 mm, 5 mm, 1 cm, 1.5 cm, 2 cm, 2.5 cm, 3 cm, 3.5 cm, 4 cm, 4.5 cm, or 4.9 cm. It is understood that the thickness of the layer can have any value that falls between any two foregoing values or within a range that is formed by any two foregoing values.
  • the thickness of the light-emitting layer can be 50 nm to 2 cm, 50 nm to 1 cm, 50 nm to 900 microns, 50 nm to 500 microns, 50 nm to 200 microns, 50 nm to 50 microns, 50 nm to 900 nm, 50 nm to 500 nm, 50 nm to 100 nm, 100 nm to 500 nm, 200 nm to 200 microns, 200 nm to 5 Attorney Docket No.11555-010WO1 UMA2023-053-01 cm, 300 nm to 5 cm, 500 nm to 5 cm, 1 micron to 5 cm, 50 microns to 5 cm, 500 microns to 5 cm, 1 cm to 5 cm and so on.
  • the substrate can have any thickness that is needed for the desired application.
  • the substrate can have a thickness of 250 microns to 50 cm, including exemplary values of 500 microns, 750 microns, 1 mm, 1 cm, 5 cm, 10 cm, 20 cm, 30 cm, 40 cm, and 45 cm. It is understood that the thickness of the substrate (transparent or non-transparent) can have any value that falls between any two foregoing values or within a range that is formed by any two foregoing values.
  • the thickness of the substrate can be 250 microns to 45 cm, 250 microns to 40 cm, 250 microns to 30 cm, 250 microns to 20 cm, 250 microns to 10 cm, 250 microns to 1 cm, 250 microns to 750 microns, 300 microns to 50 cm, 500 microns to 50 cm, 750 microns to 50 cm, 1 cm to 50 cm, 25 cm to 50 cm, and so on.
  • the one or more UV sources can be optically coupled with the light-emitting layer. Yet, in other aspects, the one or more UV light sources are optically coupled with the transparent substrate.
  • the one or more UV light sources can be optically coupled with a transparent substrate and the light-emitting layer.
  • the transparent substrate if it is present it can behave as an optical waveguide such that the light beam propagates along a longitudinal axis of the transparent substrate. Again, it is understood that the thickness of the transparent substrate can have any of the disclosed above values.
  • the light-emitting layer can have any irregular or regular shape and geometry.
  • the substrate if present, can also have any regular shape and geometry.
  • the article itself can have a regular or irregular form.
  • at least a portion of the light-emitting layer substantially conforms to at least one surface of the substrate.
  • the shape of the layer and/or substrate and/or final article can be planar, curved, concaved, convex, spherical, hemispherical, ellipsoid, having one or more edges, being substantially absent of sharp edges, or can comprise Attorney Docket No.11555-010WO1 UMA2023-053-01 sharp edges, 2 dimensional or 3 dimensional, or any combination thereof. It is further understood that the layer does not have to be fully continuous.
  • the light-emitting layer can be made as a mesh or weave or a grid-like pattern.
  • the light-emitting layer can be disposed on a specific portion of the substrate while keeping other portions free of the light-emitting layer, thus creating a desired pattern for the desired light emission.
  • the substrate is not an optical fiber.
  • the light-emitting layer is only disposed on one surface of the substrate.
  • the light- emitting layer is disposed on one or more surfaces of the substrate.
  • the light-emitting layer does not form a shell around a substrate core.
  • the one or more UV sources can operate at any wavelength in a range of 200 nm to 400 nm, including exemplary values of 210 nm, 215 nm, 220 nm, 225 nm, 230 nm, 235 nm, 240 nm, 245 nm, 250 nm, 255 nm, 260 nm, 265 nm, 275 nm, 280 nm, 285 nm, 290 nm, 295 nm, 300 nm, 305 nm, 310 nm, 315 nm, 320 nm, 325 nm, 330 nm, 335 nm, 340 nm, 345 nm, 350 nm, 355 nm, 360 nm, 365 nm, 375 nm, 380 nm, 385 nm, 390 nm, and 395 nm.
  • the wavelength can be any wavelength that falls between any two foregoing values or in a range that is formed by any two of the foregoing values.
  • the operating wavelength can be 200 nm to 380 nm, 200 nm to 350 nm, 200 nm to 300 nm, 220 nm to 380 nm, 250 nm to 300 nm, 250 nm to 280 nm, 265 nm to 300 nm, and so on.
  • each of the UV sources can be operated independently on the same or different wavelength. In certain aspects, if more than one UV source is present all UV sources operate on the same wavelength.
  • the one or more UV sources can be positioned anywhere such that the desired coupling effect is achieved.
  • the one or more UV sources can be controlled by a control unit. In such exemplary and unlimiting aspects, the control unit can adjust the operating wavelengths of the one or more UV sources over the operating time as desired.
  • one or more UV sources can operate a first predetermined wavelength that can be then changed to a second predetermined wavelength during the article operation if desired.
  • the operating wavelength can be changed and adjusted as needed.
  • the UV source can be xenon lamp, mercury lamp, laser, light- emitting diode (LED), or any combination thereof.
  • the UV source is a UV-C source.
  • the UV source is an LED.
  • the UV source can be optically coupled to a heat sink if needed.
  • the light-emitting layer comprises one or more polymer layers.
  • the plurality of light-scattering elements can be embedded within at least one polymer layer.
  • the one or more polymer layers are at least substantially UV-transparent.
  • the one or more polymer layers can exhibit a minimal absorption of the UV light in the desired range of the wavelengths.
  • the one or more polymers are transparent polymers.
  • the one or more polymers can comprise CYTOP TM , any transparent fluoropolymers, PMMA, PVC, acrylates, silicones, or any combination thereof.
  • the one or more polymer layers of the light-emitting layer can also comprise a sealing polymer.
  • this polymer can be disposed at locations that could be exposed to a delaminating environment or an environment that can negatively affect the article structure.
  • the sealing layer can be used to prevent delamination of the light-emitting layer (especially if it is disposed on the substrate).
  • the sealing layer can also be used to seal UV sources themselves or coupling routes of the UV sources with the light- emitting layer from exposure to the outside environment. In yet other aspects, the sealing layer can also be used to seal any additional electronic components, if present, in the article from the outside environment.
  • the one or more polymer layers are configured to be a host material for the plurality of the light-scattering elements that can be disposed within the polymer in any concentration or pattern.
  • the nanoparticle can be disposed within the pre-polymer solution, which can then be polymerized together with the nanoparticles.
  • the transparent polymer when used as a host, an additional transparent polymer layer can be disposed onto. Yet in still further aspects, if the transparent polymer is used as a host for the plurality of light- scattering elements no additional polymer layers are disposed onto it. It is understood, however, that the host polymer material is UV transparent and can be selected from any disclosed above polymers.
  • the nanoparticles can be first disposed on the surface, and the transparent polymer layer can be disposed onto to form the light-emitting layer.
  • the light-emitting layer can further comprise at least one of the one or more of the polymer layers that is configured to substantially prevent UV light absorption.
  • an additional layer of PTFE Teflon®
  • PTFE polytetrafluoroethylene
  • a layer of polytetrafluoroethylene (PTFE) can cure the negative effects of the silicon coating (or sealing layer) (such as a decrease in UV irradiance from the article). It was also found that the PTFE layer can prevent side emissions in areas that are not desired.
  • the positioning and composition of the one or more polymer layers can be selected based on the desired application of the article and the optical properties of each polymer layer.
  • the light-scattering elements can be present in the light-emitting layer at any concentration as desired.
  • the light- scattering elements are dispersed uniformly with the layer along any axis of the layer (length, width, and/or thickness of the light-emitting layer).
  • the light-scattering elements can form a concentration gradient along the thickness of the layer and/or length of the layer and/or width of the layer.
  • the light-emitting layer can comprise a localized dispersion of the plurality of light-scattering elements as desired.
  • the plurality of light-scattering elements is present in an amount of greater than 0 wt% to less than 100 wt% of the light-emitting layer.
  • the plurality of light-scattering elements can be present in an amount of at least 0.01 wt%, at least 0.05 wt%, at least 0.1 wt%, at least 0.5 wt%, at least 1 wt%, at least 1.5 wt%, at least 2 wt%, at least 5 wt%, at least 10 wt%, at least 20 wt%, at least 30 wt%, at least 40 wt%, at least 50 wt%, or at least 60 wt% of the light-emitting layer.
  • the concentration of the plurality of light-scattering elements can be about 2.65 ⁇ g/cm 2 to about 265 ⁇ g/cm 2 , including exemplary values of 5 ⁇ g/cm 2 , 10 ⁇ g/cm 2 , 15 ⁇ g/cm 2 , 20 ⁇ g/cm 2 , 25 ⁇ g/cm 2 , 30 ⁇ g/cm 2 , 40 ⁇ g/cm 2 , 50 ⁇ g/cm 2 , 60 ⁇ g/cm 2 , 70 ⁇ g/cm 2 , 80 ⁇ g/cm 2 , 90 ⁇ g/cm 2 , 100 ⁇ g/cm 2 , 125 ⁇ g/cm 2 , 150 ⁇ g/cm 2 , 175 ⁇ g/cm 2 , 200 ⁇ g/cm 2 , 225 ⁇ g/cm 2 , 250 ⁇ g/cm 2 , and 260 ⁇ g/cm 2
  • the concentration of the plurality of light-scattering elements can fall between any two foregoing values or in a range formed by any two foregoing values.
  • the concentration of the plurality of light-scattering elements can be 5 ⁇ g/cm 2 to about 265 ⁇ g/cm 2 , 20 ⁇ g/cm 2 to about 265 ⁇ g/cm 2 , 50 ⁇ g/cm 2 to about 265 ⁇ g/cm 2 , 100 ⁇ g/cm 2 to about 265 ⁇ g/cm 2 , 150 ⁇ g/cm 2 to about 265 ⁇ g/cm 2 , 2.65 ⁇ g/cm 2 to about 250 ⁇ g/cm 2 , 2.65 ⁇ g/cm 2 to about 200 ⁇ g/cm 2 , 2.65 ⁇ g/cm 2 to about 150 ⁇ g/cm 2 , 2.65 ⁇ g/cm 2 to about 100 ⁇ g/cm 2 , 2.
  • the silica nanoparticles can have a concentration of about 26.5 ⁇ g/cm 2 .
  • the disclosed article can be a ship hull, lenses, windows, sensors, surgical table, optical equipment, heat exchanger, medical equipment, aerospace equipment, bathroom equipment, oceanographical equipment, appliances, wound healing article, or a combination thereof.
  • the disclosed articles can be used in camera lenses, optical equipment, sensors, surgical tables, clean rooms, dental surfaces, medical surfaces, aerospace surfaces, bathroom surfaces, oceanographical surfaces, agricultural equipment, water treatment surfaces, in heat exchangers, in various appliances and equipment, and so on.
  • any of the disclosed herein articles are disinfecting. It is understood that, in some aspects, the articles are self-disinfecting. Yet, in other aspects, the articles can disinfect other objects, surfaces, and items if needed. Yet, in other aspects, the articles can disinfect other objects, surfaces, and items that are in close vicinity to the articles disclosed herein. In still further aspects, when the article is a wound healing article, the article can disinfect and treat a wound that it is applied to. It is understood that the articles disclosed herein can be or can be used anywhere wherein microbial organisms can attach and grow. Such articles can disturb or prevent the growth of microbial organisms, thereby disinfecting the desired surfaces.
  • the article can also be used in curing and advanced oxidation processes.
  • the article when the article is exposed to a biofouling environment such that at least a portion of the light-emitting layer faces the biofouling environment, the article exhibits reduced biofouling as compared to a substantially identical reference article in the absence of the light-emitting layer.
  • the article itself is anti-biofouling.
  • the articles disclosed herein can be used in marine environments to prevent the growth of biofilms on marine vehicles or oceanographic equipment.
  • disinfectant systems comprising any of the articles disclosed herein. METHODS
  • Also disclosed herein are methods of making the described above articles.
  • the methods comprise forming an article by coupling one or more UV light sources such that a light beam is side-emitted by a light-emitting layer in a direction substantially perpendicular to the direction of the light beam; wherein the light-emitting layer comprises a plurality of light-scattering elements and exhibits at least 90% transmittance; wherein the article is at least partially disinfecting and/or anti-biofouling.
  • the light-emitting layer can be disposed on a transparent or non-transparent substrate. In yet other aspects, the light-emitting layer can be at least partially embedded in the transparent layer.
  • the light-emitting layer can comprise one or more polymer layers.
  • the plurality of light-scattering elements at least partially are embedded in one or more polymer layers. It is understood that the plurality of light-scattering elements can be dispersed in the light-emitting layer as desired. In certain aspects, the plurality of light-scattering elements is uniformly dispersed in the light-emitting layer. In other aspects, the light-emitting layer comprises a concentration gradient of the plurality of light-scattering elements along the length, width, and/or depths of the light-emitting layer.
  • the light-emitting layer comprises a localized dispersion of the plurality of light-scattering elements.
  • Any of the disclosed above light-scattering elements can be used to form the disclosed herein articles.
  • the light-scattering elements disclosed herein can be of any size as disclosed above.
  • the light-scattering elements can be dissolved in a polymer solution that can be polymerized to form the desired layer.
  • the light-scattering elements can be electrostatically deposited on any surface as disclosed in the examples below.
  • the light-scattering elements embedded in the polymerized polymer to form the light-emitting layer can be electrostatically deposited on any surface as disclosed in the examples below.
  • the light-emitting layer itself can also be formed on a substrate spraying, deposition from a solution, spin coating, doctor blade coating, dip coating, 3D printing or any combination thereof.
  • the one or more polymers present in the article can be disposed by any known in the art methods. It is understood that the light- emitting layer can be formed such that it is embedded in any of the disclosed herein polymer layers, or any of the disclosed herein polymer layers can be disposed on the nanoparticles as described above.
  • the sealing layer can be applied in the desired locations by any known in the art methods. In yet still further aspects, if desired a layer PTFE can also be applied to negate undesirable effects of the sealing layer.
  • any of the disclosed herein UV sources can be used to form the desired article. Any of the disclosed above couplings of the one or more UV sources in the article can be utilized.
  • Attorney Docket No.11555-010WO1 UMA2023-053-01 Also disclosed herein are methods comprising; forming any of the disclosed herein articles; exposing the article to a biofouling environment such that the light-emitting layer at least partially faces the biofouling environment, passing a light beam from the one or more UV-light sources to initiate side-emission of the UV light, and reducing biofouling at at least a portion of a surface of the article that is exposed to the biofouling environment.
  • the article is self- disinfecting.
  • the article is anti-biofouling.
  • a method comprising: exposing any of the disclosed herein articles to a biofouling environment such that the light-emitting layer at least partially faces the biofouling environment, passing a light beam from the one or more UV-light sources to initiate a side emission of the UV light, and reducing biofouling at at least a portion of a surface of the article that is exposed to the biofouling environment.
  • EXAMPLE 1 In this example, disclosed is an approach where UV light has glowed from the inside of windows to prevent biological attachment and growth.
  • Glass Attorney Docket No.11555-010WO1 UMA2023-053-01 substrates such as windows can be modified to externally emit UV light and eliminate biological growth on their surface.
  • nanoparticle-enabled waveguides are formed. UVC light (265 nm), launched from an LED, travels through the glass core and is scattered by the nanoparticles on the surface, resulting in side-emission into its surrounding environment (water/air). ⁇ When total internal reflection (TIR) occurs within a waveguide, an evanescent wave, or electromagnetic disturbance, is generated through the sides of the substrate.
  • TIR total internal reflection
  • SEOFs side-emitting optical fibers
  • a traditional optical fiber with highly scattering particles sica spheres >200 nm in diameter
  • a UV 265 nm LED to the fiber.
  • SEOFs can effectively inactivate planktonic bacteria (2.9 log inactivation of Escherichia coli at a delivery dose of 15 mJ/cm 2 ) and prevent bacteria growth on surfaces (inhibition zone of 3 cm at a delivery dose of ⁇ 4.3 mJ/cm 2 ).
  • the side-emitting layers can have any desired geometry or can be formed on any surface having the desired geometry without any limitations.
  • the UVC emitting glass (UEG) was fabricated to emit UV light throughout its length (FIG.1A).
  • the UEG was deployed in a marine environment for 20 days to assess the ability of UEGs to prevent biofilm when compared to a similar non-UEG control.
  • the biofouling- resistant device and methods may be incorporated into any transparent window. For example, in optical equipment for cameras, signal transmission (UV through IR) and detection equipment, as well as window surfaces.
  • the device and method disclosed herein may be adapted for biofilm prevention on any surface, both in marine and other ecosystems/environments.
  • the biofouling- resistant device comprises a transparent media, such as glass, having an outer surface with a light dispersive coating deposited thereon.
  • the light dispersive Attorney Docket No.11555-010WO1 UMA2023-053-01 coating may include a layer of silica nanoparticles ranging in size from at least 50 nm to at least 100 nm to at least 200 nm in diameter.
  • the silica nanoparticles may be spherical.
  • a UV light source is optically connected to the transparent media.
  • an LED can be optically connected to the transparent media.
  • the light source may further include thermal management solutions, such as an Al backing plate and/or heat sink connected to the LED. Other thermal management techniques, as known in the art, may be used.
  • the dispersive coating disperses UV light emitted from the UV light source onto the outer surface of the transparent media, thereby reducing biofouling.
  • the UV light source can emit light in wavelengths between about 250 nm and about 280 nm, and in other aspects, at about 265 nm.
  • the concentration of silica nanoparticles may be from about 2.65 ⁇ g/cm 2 to about 265 ⁇ g/cm 2 . In yet other aspects, the silica nanoparticles can have a concentration of about 26.5 ⁇ g/cm 2 .
  • An optional silicone binder coating may overlay the light-dispersive coating to protect the light-dispersive coating.
  • the biofouling-resistant devices may be made by providing a transparent media having an outer surface. The outer surface may be coated through a technique such as electrostatic deposition with a light dispersive coating, such as aminated silica nanoparticles. The UV light source is optically connected to the transparent media, either before or after the coating step.
  • the LED can be optically connected to an edge of the transparent media.
  • the biofouling-resistant device may be incorporated into a marine environment that is highly prone to biofouling, such as a window on the bridge of a marine vessel. Besides windows and portholes on marine vessels, the biofouling-resistant device and methods may be incorporated into any transparent window. For example, in optical equipment for cameras, signal transmission (UV through IR) and detection equipment, as well as window surfaces. Additionally, through slight modifications to this technology (towards thin film), the device and method disclosed herein may be adapted for biofilm prevention on any surface, both in marine and other ecosystems/environments.
  • UV-emitting glass UV transparent quartz slides measuring 24 x 110 mm and 2 mm thick were modified to emit UV light through a three-step method. Step 1 involved cleaning the slides at room temperature by immersing them in acetone (99.5%) and sonicating the solution for 10 min to remove any deposits from the exposed surfaces. Step 2 included the application of scattering nanoparticles onto the cleaned slides by electrostatic deposition mechanism.
  • Aminated silica spheres suspended in ethanol with a diameter of 200 nm were selected due to the low absorptivity and high scattering coefficient at UV 265 nm. Positively charged aminated spheres facilitated the attachment to the negatively charged glass slide surface.
  • the nanoparticle suspension was sonicated for 10 minutes before application. Approximately 700 ⁇ L of the suspension was gently pipetted onto the slide to uniformly cover the 26.5 cm 2 surface area of the slide before drying for 2 hours.
  • UEGs with different mass coverage ( ⁇ g/cm 2 ) of nanoparticles on the slides were fabricated by diluting the nanoparticle suspension with Ethyl Alcohol 100% (Decon Laboratories, Inc. PA).
  • the slide was coated with a UV transparent polymer by semi-print screen technique. Following sonication for 10 minutes, 300 ⁇ 20 ⁇ L polymer (for example, Cyclic Transparent Optical Polymer (CYTOPTM) (AGC Chemicals, USA)) was dragged along the exposed facet of the glass slide and dried at room temperature overnight. [0128] . A minimum coating thickness was desired while ensuring complete coverage of the substrate and nanoparticles.
  • CYTOPTM Cyclic Transparent Optical Polymer
  • CYTOP is a fluoropolymer characterized by its amorphous structure, allowing for remarkable transparency (>95% for 1 mm) over a wide spectral range (200–2000 nm), and is well-suited for functioning as an optical thin film coating.
  • the thickness of the coating material was measured by AFM profilometry using a Jupiter XR Atomic Force Microscopy (AFM) (Oxford Asylum Research, UK) across a scratch made by a brass pin on the coating layer. When scanning, measurements of the material derived from scratching were avoided by selecting areas free of debris when possible.
  • the instrument was operating in tapping mode using Super- Sharp PointProbe-Plus®- NCHR Silicon tips (NANOSENSORSTM, Switzerland).
  • Optical transparency and UV emission profiles were subsequently characterized for the fabricated UEGs.
  • the optical transparency of the slides was measured by the U.S. Naval Research Laboratory (NRL) by positioning a collimated light source in front of the substrate followed by a detector behind it. Measurements were carried out in the Vis to NIR spectra (400 – 2500 nm) using Flame and NIR Quest spectrometers (Ocean Insight, USA) working in tandem.
  • the light sources used in the measurements were provided by Ocean Insight light sources (DH-2000-FHS-DUV- TTL for Vis and HL-2000-HP-FHSA for NIR, respectively), directed onto the slide using a sample 74-ACH adjustable collimating lens holder, modified with custom- made 3D printed panel brace and 74-UV collimating lenses.
  • the intensity of light passing through the slides was collected and recorded using the OceanView software package, and the %Transmission was calculated during data processing using the MATLAB software package using control (uncoated) slides for background signals.
  • Visual Resolving Power evaluations were conducted using a USAF 1951 Optical Calibration Target printed at 8.5” x 11” scale. Comparisons are made to appropriate uncoated blank.
  • UVC emission profile measurements were conducted using a spectrophotoradiometer (AvaSpec-2048L, Avantes, Louisville, CO USA), calibrated over the wavelength range of 200 to 1100 nm.
  • UEGs were placed in a slide holder case (section 2.3.1) in a perpendicular position to the UV LED lamp.
  • the UV irradiance ( ⁇ W/cm 2 ) was measured along the length and perpendicular distance from the UEG surface by placing the spectrophotoradiometer’s sensor tip (5 mm 2 ) normal to the surface at a 1 mm distance. Intensity was measured at distances of 1, 3, 5, 7, and 9 cm from the UV lamp (for example, LED).
  • the total irradiance was obtained by integrating the output spectrum between 240 nm and 300 nm.
  • Attorney Docket No.11555-010WO1 UMA2023-053-01 Triplicate measurements were taken at each position along independent UEGs. The output intensity was corrected for the dark data for correct full-width half maximum (FWHM) calculations.
  • the reflectance of light by the benchtop was measured by inverting the spectroradiometer tip away from the light source and normal to the benchtop surface. No signal was measured, indicating that the surrounding material had no influence on the light distribution profile. [0132]
  • the absorbance of air and light reflectivity of the benchtop were negligible and should not influence the light distribution profile. However, the light attenuation profile would change when the UEGs are placed in water.
  • Submersion - Case design The submersion cases were 3D-printed by UMass Advanced Digital Design and Fabrication (ADDFab) 3D printing facilities.
  • the material used for the case printing was nylon-12 (PA2200) with a density (laser sintered) of 930 kg/m 3 and certified for biological tests (USP class: VI).
  • Each case contained six chambers housing two control slides and 4 UEG (nanoparticles concentration: 26.5 ⁇ g/cm 2 ) (FIG.2).
  • the controls included polymer-only slides with no UV.
  • Each chamber dimension was approximately 25 mm x 3 mm x 100 mm.3D-printed side brackets secured the water irradiance against one side of the chamber so that only one side of the slides was exposed to the marine environment. Non-exposing sides of all slides were coated with polymer.
  • Coupling UV LED to UEG The 3D-printed cases contained specific areas designed to accommodate the LED strip, aluminum backing, heat sink, and electrical connections and wiring (FIG.2). Strips of four UV LEDs with 30-degree lenses and emission peak of 265 nm were purchased from Violumas, San Diego, CA. The maximum forward current and forward voltage were 700 mA and 24 V, respectively. The LED strip was screwed to the aluminum backing and placed in the light housing space.
  • a butt-coupling approach was used between LED and UEGs.
  • the UEGs were secured inside the light engine by a silicone binder.
  • the LED set up produces up to 2-4 J/s of heat during the submersion.
  • the marine environment was used as the heat sink.
  • four 22 mm x 22 mm x 7 mm anodized aluminum heatsinks (Easycargo, Amazon, Seattle, WA, USA) were attached to the Al backing Attorney Docket No.11555-010WO1 UMA2023-053-01 to ensure proper semiconductor cooling.
  • a fan (HT 900, Honeywell, Charlotte, NC, USA) was directed to the LED to further dissipate heat.
  • the extracted biofilm was suspended in a 10 mL sterile phosphate buffer solution (PBS) to prevent osmotic shock and dispersed via combined action of vortex-ultrasound- vortex (each for 1 min).
  • the resulting suspension was designated as BS (biofilm suspension).
  • PBS sterile phosphate buffer solution
  • the resulting suspension was designated as BS (biofilm suspension).
  • the suspension was incubated at room temperature for 1h. Subsequently, the suspension was centrifuged at 10,000 ⁇ g for 10 minutes, and the pellet was resuspended in another 20 mL buffer solution. Once again, the sample was vortexed and centrifuged as described above. No dilution occurred during washing. [0143] The harvested cells were suspended in a 2 mL buffer solution and vortexed for 1 min.
  • GFP Green fluorescent protein
  • RFP red fluorescent protein
  • the quantification of total proteins in each sample fraction was performed using QubitTM Protein Assay Kit (Invitrogen, USA) and a Qubit R 2.0 Fluorometer without protein isolation.
  • the QIAamp Viral RNA Kit (Qiagen, USA) was used.
  • the QIAamp Viral RNA Mini Kit can extract small quantities of viral RNA and cellular DNA if both are present in the sample.
  • the biofilm suspension (900 ⁇ L) was concentrated by centrifugation at 10,000 ⁇ g for 10 minutes. Supernatant was decanted. Phosphate buffer solution was added to the pellet to a final volume of 140 ⁇ L.
  • the subsequent extraction by the QIAamp Viral RNA Kit was done according to the manufacturers protocol.
  • FIGs.15A-15B show top view images of glass surface coated with only polymer (FIG 15A (a1)) and nanoparticles + polymer (FIG 15B (b1) as well as the respective corresponding cross-sectional profiles (FIG 16A (a2) and FIG 16B (b2)).
  • the method of scratching is used in analyzing the polymer thickness leaves accumulated residue. Therefore, the reported polymer thickness is the measurement after the residue (test) minus the Attorney Docket No.11555-010WO1 UMA2023-053-01 measurement before the residue (glass). Based on the cross-sectional profiles, the mean thickness of only polymer and nanoparticles + polymer was 151 ⁇ 9 nm and 422 ⁇ 83 nm, respectively. [0148] In this example, the goal was to minimize the polymer thickness applied to the substrate while ensuring complete coverage of the substrate and nanoparticles. The polymer thickness should not have a strong effect on the UV performance of the UEGs due to the high transparency of >95% for 1 mm thickness of material.
  • ⁇ is a function of the optical and physical properties of the glass and the surface coating.
  • SiO2 has low absorption at UVC range due to its insulation characteristics.
  • the photon energy of 4.67 eV in 265 nm Attorney Docket No.11555-010WO1 UMA2023-053-01 wavelength cannot be absorbed and will not be able to excite enough of the valence band electrons to jump into the conduction band.
  • FIG.3B illustrates the UVC profile after a polymer layer was added to the slides.
  • more Attorney Docket No.11555-010WO1 UMA2023-053-01 than a 50% decrease in UV irradiance was observed for UEG prepared with a nanoparticle concentration of 2.65 ⁇ g/cm 2 .
  • Such decrement can result from decreased interaction between nanoparticle and glass slide after the polymer is introduced and was discernible at lower concentrations of nanoparticles.
  • FIG.5 depicts the UV irradiance profile and spectral output for the final configuration of UEGs.
  • FIGs.4A-4B presents the Vis-NIR transmission spectra of glass slides that were coated with different concentrations of nanoparticles, both with and without polymer.
  • polymer coating did not increase the transmission of the slides with concentrations of 2.65 and 265 ⁇ g/cm 2 of nanoparticles.
  • increasing the thickness of the coating results in an extended optical path length, that can therefore lead to a reduction in transparency.
  • thicker coatings would significantly decrease the UV transparency.
  • the polymer has >95% transparency for a path length of 1 mm, changes in UV emission due to polymer thickness were negligible.
  • the light transmittance of the slides used for submersion (concentration of nanoparticles: 26.5 ⁇ g/cm 2 ) in the Vis region was 88 ⁇ 1.6% without polymer coating and 100.4 ⁇ 0.6% with the polymer coating.
  • Light transmission in the NIR region was 101 ⁇ 0.6% without polymer coating and 99.4 ⁇ 1.3% with polymer coating. Data exceeding 100 % are attributed to experimental errors in the instrumentation.
  • FIGS.6A-6B illustrates the photographs of the control slides and UEGs that were exposed to continuous UVC radiation after being submerged for 20 days.
  • Visual assessment results indicated a reduction of over 92% in biofilm coverage on UEGs compared to the control slides.
  • the slides modified with scattering centers delivered more than 7.7 times the UVC dose and achieved 13.7-fold less biofilm coverage compared to the control slides.
  • Most of the growth was micro biofouling, green algae and amphipod tubes.
  • Quantification of biofilm growth developed on slides as CFUs are presented in FIGS.7A-7C.
  • the culturable cells attached to the surface of each slide were quantified as CFU and are presented in FIG.7A.
  • the control slides exhibited CFU counts of about 1000 ⁇ 190, 700 ⁇ 280, and 600 ⁇ 310 CFU/ cm 2 for p1, p2, and p3 sections, respectively.
  • the UEGs showed significantly lower CFU counts, with only 10 ⁇ 2.7 CFU/ cm 2 for p1, 12 ⁇ 6.6 CFU/ cm 2 for p2, and 16 ⁇ 5.5 CFU/ cm 2 for p3.
  • the number and proportion of dead cells in biofilm grown on UEG was also lower than that of control slides (FIG.7C).
  • the live:dead ratio was 82:1 and 25:1 for biofilm grown on UEG and control slides, respectively. This can result from the mode of action of the LIVE/DEAD Baclight stains being incongruous with the UV inactivation mechanism.
  • the LIVE/DEAD BacLight method allows for the detection of cell states beyond just live and dead cells. This includes the identification of live injured cells that are unable to grow on agar plates.
  • Germicidal UVC prevents the buildup of bacterial biofilms by breaking the chemical bonds between DNA and RNA polymers within microorganisms, disrupting the genetic code, and preventing DNA from replicating.
  • DNA and proteins are two of the main molecules identified in natural marine biofilms that are essential for biofilm growth and survival. The total DNA unbound and bound protein concentrations were determined on each UEG and control slide and are illustrated in FIG.8.
  • the mean value of total DNA concentration for control and UEG slides were 1.6 ⁇ 0.33 ng/cm 2 and 0.2 ⁇ 0.1 ng/cm 2 , respectively. These results align with the number of CFU observed in both control and UEG slides.
  • UVC radiation particularly targets nucleic acid molecules, and it interacts with bacterial DNA to inhibit growth, reproduction, and the formation of biofilms. It is worth noting that an increased cell density in the biofilm corresponds to a greater concentration of DNA.
  • the concentration of bound proteins in the control slides was 0.17 ⁇ 0.05 ⁇ g/cm 2 . However, bound protein concentration was below detection in the UEGs. Additionally, the concentration of unbound proteins was below detection on all slides.
  • UEG can be used for disinfection of transparent surfaces such as windows of flotation spheres and moored buoys, camera lenses, and sensors for oceanographical, agricultural, water treatment, and process design applications.
  • UEGs can be manufactured on a commercial scale, considering the surrounding materials to be UV-resistant. Overall, this study contributes valuable insights into the field of surface engineering and sets the stage for further advancement in the realm of antimicrobial coatings and treatments.
  • EXAMPLE 6 UV EMITTING TRANSPARENT SURFACE FOR BIOFILM PREVENTION
  • UV-emitting glass (UEG) slides and lenses were fabricated by first dipping the slides in acetone for cleaning. SiO2 nanoparticles were then coated onto the slides by an electrostatic deposition mechanism. Finally, the slides were coated with a UV-transparent polymer.
  • FIG.9 shows a schematic of each layer of the slides.
  • FIGS.10A-10C shows photographs of the slides before and after coating.
  • the UV emission profiles of the UEG lenses can be measured at multiple wavelengths.
  • FIG.11 shows the UV measurement setup for a 100 mm (diameter) x 6 mm (thickness) lens.
  • FIG.12 shows an example case design for the submersion of UEGs in a marine environment.
  • FIGS.13A-13F show the UV emission profiles of UEG at 275 nm.
  • FIGs. 13E-13F show the light propagation from 6 different LEDs positioned along the circumference of the lens.
  • FIGS.14A-14C show the UV emission profiles of UEG at 265 nm. The UEG used to generate both emission profiles was a 100 mm (diameter) x 6 mm (thickness) lens.
  • FIGS.17A-17B and TABLE 2 demonstrate that silicone sealing decreases UV irradiance from glass slides.
  • FIG.18 shows that the materials with high absorption coefficients have high refractive indices.
  • This study used low refractive index-polymer to resolve the negative effect of silicone sealing on UV irradiance from glass slides. For this purpose, polytetrafluoroethylene (PTFE) with a refractive index of 1.356 was used.
  • PTFE polytetrafluoroethylene
  • the CYTOP polymer coating was carefully applied in a bottom-to-top direction, preventing any potential scrubbing or dragging of the PTFE on the slide surface. After coating, the slides were left to dry overnight. [0178] 4) The back side of the slide was coated with a PTFE layer by pipetting 40 ⁇ L of polymer onto the top 0.6 cm section of the bare surface and dried by indirect heating. [0179] 5) The back side of the slide from step 4 was coated with CYTOP polymer according to the method outlined in step 4. [0180] The PTFE coating is highly efficient in preventing UV light from being absorbed by the silicone sealant.
  • FIGS.19A-19B depict the PTFE-coated slides.
  • FIG.20 and TABLE 3 demonstrate that the PTFE coating omitted the adverse effect of silicon on UV irradiance.
  • Distance (cm) Before silicone sealing ( ⁇ W/cm 2 ) After silicone sealing ( ⁇ W/cm 2 ) Attorney Docket No.11555-010WO1 UMA2023-053-01 Distance (cm) Before silicone sealing ( ⁇ W/cm 2 ) After silicone sealing ( ⁇ W/cm 2 ) [0181]
  • the study next tested the submersion of the UEGs in a marine environment. Cases were submerged at Port Canaveral, Florida, United States, for 20 days.
  • FIGS.21A-21C show the experimental setup.
  • the cases used a UV input power of 16.8 W, a UV wavelength of 265 nm, and continuous irradiation mode.
  • FIG.22 shows a significant inhibitory effect (92%) of UEGs on the biofilm growth based on visual assessment. Overall, there was a 98.28% decrease in biofilm coverage based on CFU, as shown in FIG.23.
  • the study tested the submersion of the UEGs in laboratory conditions. The UEGs were submerged with either Pseudomonas aeruginosa or mixed marine bacteria for 8 days at a temperature of 16-19°C.
  • FIG.24 shows the experimental setup.
  • FIG.25 shows the UV emission profiles of UEG slides at multiple wavelengths. The slides used were 24 mm (W) x 110 mm (L) x 2 mm (T).
  • FIG.26 shows the results of UEGs submerged with Pseudomonas bacteria. The highest Log Reduction Value (LRV) was observed at 265 nm. The wavelength effectiveness trend was: 265 nm > 280 nm > 310 nm > 365 nm.
  • FIG.27 shows the results of UEGs submerged with mixed marine bacteria.265 nm showed the highest LRV of 3.04. The wavelength effectiveness trend was: 265 nm > 280 nm > 310 nm > 365 nm. Viable cell count decreased from Attorney Docket No.11555-010WO1 UMA2023-053-01 control slides to UEGs. This is an indication of biofilm prevention by cell detachment.
  • FIG.28 shows electrical power per order. Understanding the electrical energy requirement is crucial for any light-based technology.
  • FIG.29 shows optical coherence tomography (OCT) images of biofilm.
  • OCT optical coherence tomography
  • FIG.30 shows measuring biofilm thickness at the areas covered by biofilm. The thickness variation was high (0 to 150 ⁇ m in UEG, 0 to 298 ⁇ m in control slides).
  • FIG.31 compares the effectiveness of UEG with external UV irradiation. Among these studies, UEG showed the highest LRV with minimum UV irradiance value. Only one other study showed the highest LRV with lower irradiance than UEG (Bak, J.; Ladefoged, S. D.; Tvede, M.; Begovic, T.; Gregersen, A. Disinfection of Pseudomonas Aeruginosa Biofilm Contaminated Tube Lumens with Ultraviolet C Light Emitting Diodes.
  • Example 1 An article comprising (a) a light-emitting layer; and (b) one or more UV light sources coupled within the article such that a light beam is side- emitted by the light-emitting layer in a direction substantially perpendicular to a direction of the light beam; wherein the light-emitting layer comprises a plurality of light-scattering elements and exhibits at least 90% transmittance.
  • Example 2 The article of any examples herein, particularly Example 1, wherein the plurality of light-scattering elements comprise a plurality of nanoparticles.
  • Example 3 The article of any examples herein, particularly Example 1 or 2, wherein the one or more UV light sources are optically coupled with the light- emitting layer.
  • Example 4 The article of any examples herein, particularly Examples 1- 3, wherein the plurality of light-scattering elements comprise silica nanoparticles having a size of 50 nm to 500 nm.
  • Example 5 The article of any examples herein, particularly Examples 1- 4, wherein the light-emitting layer is positioned on a transparent or non-transparent substrate.
  • Example 6 The article of any examples herein, particularly Example 5, wherein the substrate is transparent, and the light-emitting layer is (i) disposed on a surface of the substrate, and/or (ii) at least partially embedded into a body of the transparent substrate adjacent to the surface of the substrate and wherein the plurality of light-scattering elements comprise one or more of a plurality of particles, defects, air bubbles, or a combination thereof.
  • Example 7 The article of any examples herein, particularly Example 5 or 6, wherein the one or more UV light sources are optically coupled with the transparent substrate and/or the light-emitting layer.
  • Example 8 The article of any examples herein, particularly Example 7, wherein the transparent substrate behaves as an optical waveguide such that the Attorney Docket No.11555-010WO1 UMA2023-053-01 light beam propagates along a longitudinal axis of the transparent substrate and wherein the transparent substrate has a thickness of 250 microns to 50 cm.
  • Example 9 The article of any examples herein, particularly Examples 1- 8, wherein the one or more UV light sources operate at the same or different wavelengths.
  • Example 10 The article of any examples herein, particularly Examples 1- 9, wherein the one or more UV light sources comprise a light emitting diode (LED).
  • LED light emitting diode
  • Example 11 The article of any examples herein, particularly Examples 1- 10, wherein the light-emitting layer has a thickness of 50 nm to 5 cm.
  • Example 12 The article of any examples herein, particularly Examples 5- 11, wherein the substrate has a regular or irregular geometry.
  • Example 13 The article of any examples herein, particularly Examples 5- 12, wherein at least a portion of the light-emitting layer substantially conforms to at least one surface of the substrate.
  • Example 14 The article of any examples herein, particularly Examples 7- 13, wherein the one or more UV light sources are optically coupled at any location with the transparent substrate and/or the light-emitting layer.
  • Example 15 The article of any examples herein, particularly Examples 1- 14, wherein the light-emitting layer comprises one or more polymer layers.
  • Example 16 The article of any examples herein, particularly Example 15, wherein one of the one or more polymer layers is a sealing layer.
  • Example 17 The article of any examples herein, particularly Example 15 or 16, wherein one of the one or more of the polymer layers is configured to substantially prevent UV light absorption.
  • Example 18 The article of any examples herein, particularly Examples 1- 17, wherein the article is a ship hull, lenses, windows, sensors, surgical table, optical equipment, heat exchanger, medical equipment, aerospace equipment, bathroom equipment, oceanographical equipment, appliances, wound healing article, or a combination thereof.
  • Example 19 The article of any examples herein, particularly Examples 1- 18 wherein when the article is exposed to a biofouling environment such that at least a portion of the light-emitting layer faces the biofouling environment, the article exhibits reduced biofouling as compared to a substantially identical reference article in the absence of the light-emitting layer.
  • Example 20 The article of any examples herein, particularly Examples 1- 19, wherein the article is disinfecting.
  • Example 21 The article of any one of Examples 1-20, wherein the article is anti-biofouling.
  • Example 22 A disinfectant system comprising the article of any examples herein, particularly Examples 1-21.
  • Example 23 A method of comprising: forming an article by coupling one or more UV light sources such that a light beam is side-emitted by a light-emitting layer in a direction substantially perpendicular to the direction of the light beam; wherein the light-emitting layer comprises a plurality of light-scattering elements and exhibits at least 90% transmittance; wherein the article is at least partially disinfecting and/or anti-biofouling.
  • Example 24 The method of any examples herein, particularly Example 23, wherein the light-emitting layer is disposed on a transparent or non-transparent substrate.
  • Example 25 The method of any examples herein, particularly Examples 23-24, wherein the light-emitting layer comprises one or more polymer layers.
  • Example 26 The method of any examples herein, particularly Example 25, wherein the plurality of light-scattering elements at least partially are embedded in one or more polymer layers.
  • Example 27 The method of any examples herein, particularly Examples 23-26, wherein the plurality of light-scattering elements are uniformly dispersed in the light-emitting layer.
  • Example 28 The method of any examples herein, particularly Examples 23-27, wherein the light-emitting layer comprises a concentration gradient of the Attorney Docket No.11555-010WO1 UMA2023-053-01 plurality of light-scattering elements along a length, width, and/or depths of the light-emitting layer.
  • Example 29 The method of any examples herein, particularly Examples 23-28, wherein the light-emitting layer comprises a localized dispersion of the plurality of light-scattering elements.
  • Example 30 The method of any examples herein, particularly Examples 23-29, wherein the plurality of light-scattering elements comprise a plurality of nanoparticles.
  • Example 31 The method of any examples herein, particularly Examples 24-30, wherein the light-emitting layer is formed by embedding a plurality of nanoparticles, forming defects, air bubbles, or a combination thereof within at least a portion of a surface of the substrate, wherein the substrate is transparent.
  • Example 32 The method of any examples herein, particularly Examples 25-31, wherein one of the one or more polymer layers is a sealing layer.
  • Example 33 The method of any examples herein, particularly Examples 25-32, wherein at least one of the one or more of the polymer layers is configured to substantially prevent UV light absorption.
  • Example 34 The method of any examples herein, particularly Examples 23-33, wherein the plurality of light-scattering elements comprise a plurality of silica nanoparticles having a size of 50 nm to 500 nm.
  • Example 35 The method of any examples herein, particularly Examples 23-34, wherein the one or more UV light sources comprise an LED.
  • Example 36 The method of any examples herein, particularly Examples 23-35, wherein the one or more UV light sources operate at the same or different wavelengths.
  • Example 37 The method of any examples herein, particularly Examples 23-36, wherein the light-emitting layer has a thickness of 50 nm to 5 cm.
  • Example 38 The method of any examples herein, particularly Examples 24-37, wherein the one or more UV light sources are optically coupled at any location with the transparent substrate and/or the light-emitting layer.
  • Attorney Docket No.11555-010WO1 UMA2023-053-01 [0229]
  • Example 39 The method of any examples herein, particularly Examples 23-38, wherein the article is a ship hull, lenses, windows, sensors, surgical table, optical equipment, heat exchanger, medical equipment, aerospace equipment, bathroom equipment, oceanographical equipment, appliances, wound healing article, or a combination thereof.
  • Example 40 A method comprising: forming an article of any examples herein, particularly Examples 1-22; exposing the article to a biofouling environment such that the light-emitting layer at least partially faces the biofouling environment, passing a light beam from the one or more UV-light sources to initiate a side emission of the UV light, and reducing biofouling at at least a portion of a surface of the article that is exposed to the biofouling environment.
  • Example 41 A biofouling-resistant device, comprising: a transparent media having an outer surface, the outer surface having a light dispersive coating deposited thereon; and a UV light source optically connected to the transparent media; whereby the dispersive coating disperses UV light emitted from the UV light source onto the outer surface of the transparent media thereby reducing biofouling.
  • Example 42 The device of any examples herein, particularly Example 41, wherein the UV light source emits light in wavelengths between about 250 nm and about 280 nm.
  • Example 43 The device of any examples herein, particularly Example 41 or 42, wherein the UV light source emits light in wavelength at about 265 nm.
  • Example 44 The device of any examples herein, particularly Examples 41-43, wherein the light dispersive coating comprises silica nanoparticles.
  • Example 45 The device of any examples herein, particularly Example 44, wherein the silica nanoparticles comprise diameters having at least 50 nm.
  • Example 46 The device of any examples herein, particularly Example 45, wherein the silica nanoparticles comprise diameters having at least 100 nm.
  • Example 47 The device of any examples herein, particularly Example 46, wherein the silica nanoparticles comprise diameters having at least 200 nm.
  • Example 48 The device of any examples herein, particularly Example 47, wherein the silica nanoparticles have a concentration from about 2.65 ⁇ g/cm 2 to about 265 ⁇ g/cm 2 .
  • Example 49 The device of any examples herein, particularly Example 48, wherein the silica nanoparticles have a concentration of about 26.5 ⁇ g/cm 2 .
  • Example 50 The device of any examples herein, particularly Example 41-49, further comprising a silicone binder coating overlaying the light dispersive coating.
  • Example 51 The device of any examples herein, particularly Example 41-50, wherein the UV light source is an LED.
  • Example 55 The method of any examples herein, particularly Example 52-54, wherein the UV light source is configured and arranged to emit light in wavelengths between about 250 nm and about 280 nm.
  • Example 56 The method of any examples herein, particularly Example 52-55, wherein the UV light source emits light in wavelength at about 265 nm.
  • Example 57 The method of any examples herein, particularly Example 52-56, wherein the light dispersive coating comprises silica nanoparticles from about 50 nm in diameter to about 200 nm in diameter.
  • Example 58 The method of any examples herein, particularly Example 57, wherein the silica nanoparticles have a concentration from about 2.65 ⁇ g/cm 2 to about 265 ⁇ g/cm 2 .
  • Example 59 The method of any examples herein, particularly Example 58, wherein the silica nanoparticles have a concentration of about 26.5 ⁇ g/cm 2 .
  • Example 60 The method of any examples herein, particularly Example 52-59, wherein the UV light source is an LED.

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Abstract

L'invention concerne un article comprenant (a) une couche électroluminescente ; et (b) une ou plusieurs sources de lumière UV couplées à l'intérieur de l'article de telle sorte qu'un faisceau lumineux est émis latéralement par la couche électroluminescente dans une direction sensiblement perpendiculaire à une direction du faisceau lumineux ; la couche électroluminescente comprenant une pluralité d'éléments de diffusion de lumière et présentant une transmittance d'au moins 90 %. L'invention concerne également des procédés de fabrication et d'utilisation de celui-ci.
PCT/US2024/033043 2023-06-08 2024-06-07 Verre émettant des ultraviolets et son procédé de fabrication Ceased WO2024254473A1 (fr)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150194579A1 (en) * 2012-09-21 2015-07-09 Postech Academy-Industry Foundation Color converting element and light emitting device including the same
WO2019040358A1 (fr) * 2017-08-22 2019-02-28 Corning Incorporated Article en verre avec couche de codage de position spatiale de conversion de lumière transparente
WO2020236549A1 (fr) * 2019-05-23 2020-11-26 Corning Incorporated Lunettes à décalage de couleur négative et plaques de guidage de lumière
US20210122667A1 (en) * 2018-10-01 2021-04-29 Paul K. Westerhoff Uv-c wavelength radially emitting particle-enabled optical fibers for microbial disinfection
US11035993B2 (en) * 2015-08-14 2021-06-15 S.V.V. Technology Innovations, Inc Illumination systems employing thin and flexible waveguides with light coupling structures

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150194579A1 (en) * 2012-09-21 2015-07-09 Postech Academy-Industry Foundation Color converting element and light emitting device including the same
US11035993B2 (en) * 2015-08-14 2021-06-15 S.V.V. Technology Innovations, Inc Illumination systems employing thin and flexible waveguides with light coupling structures
WO2019040358A1 (fr) * 2017-08-22 2019-02-28 Corning Incorporated Article en verre avec couche de codage de position spatiale de conversion de lumière transparente
US20210122667A1 (en) * 2018-10-01 2021-04-29 Paul K. Westerhoff Uv-c wavelength radially emitting particle-enabled optical fibers for microbial disinfection
WO2020236549A1 (fr) * 2019-05-23 2020-11-26 Corning Incorporated Lunettes à décalage de couleur négative et plaques de guidage de lumière

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