WO2019159171A1 - Lecteur de motif et/ou de spectres et ses utilisations - Google Patents

Lecteur de motif et/ou de spectres et ses utilisations Download PDF

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Publication number
WO2019159171A1
WO2019159171A1 PCT/IL2019/050179 IL2019050179W WO2019159171A1 WO 2019159171 A1 WO2019159171 A1 WO 2019159171A1 IL 2019050179 W IL2019050179 W IL 2019050179W WO 2019159171 A1 WO2019159171 A1 WO 2019159171A1
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WO
WIPO (PCT)
Prior art keywords
pattern
spectra
poly
fluorescent carbon
inkjet ink
Prior art date
Application number
PCT/IL2019/050179
Other languages
English (en)
Inventor
Michael SHTEIN
Amit HAVIV
Shai GERTNER
Yoni Engel
Original Assignee
Dotz Nano Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Dotz Nano Ltd filed Critical Dotz Nano Ltd
Publication of WO2019159171A1 publication Critical patent/WO2019159171A1/fr
Priority to IL276184A priority Critical patent/IL276184A/en

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B42—BOOKBINDING; ALBUMS; FILES; SPECIAL PRINTED MATTER
    • B42D—BOOKS; BOOK COVERS; LOOSE LEAVES; PRINTED MATTER CHARACTERISED BY IDENTIFICATION OR SECURITY FEATURES; PRINTED MATTER OF SPECIAL FORMAT OR STYLE NOT OTHERWISE PROVIDED FOR; DEVICES FOR USE THEREWITH AND NOT OTHERWISE PROVIDED FOR; MOVABLE-STRIP WRITING OR READING APPARATUS
    • B42D25/00—Information-bearing cards or sheet-like structures characterised by identification or security features; Manufacture thereof
    • B42D25/30—Identification or security features, e.g. for preventing forgery
    • B42D25/36—Identification or security features, e.g. for preventing forgery comprising special materials
    • B42D25/378—Special inks
    • B42D25/387—Special inks absorbing or reflecting ultraviolet light
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/02—Details
    • G01J3/0264—Electrical interface; User interface
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/02—Details
    • G01J3/0272—Handheld
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28—Investigating the spectrum
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28—Investigating the spectrum
    • G01J3/2823—Imaging spectrometer
    • G—PHYSICS
    • G07—CHECKING-DEVICES
    • G07D—HANDLING OF COINS OR VALUABLE PAPERS, e.g. TESTING, SORTING BY DENOMINATIONS, COUNTING, DISPENSING, CHANGING OR DEPOSITING
    • G07D7/00—Testing specially adapted to determine the identity or genuineness of valuable papers or for segregating those which are unacceptable, e.g. banknotes that are alien to a currency
    • G07D7/06—Testing specially adapted to determine the identity or genuineness of valuable papers or for segregating those which are unacceptable, e.g. banknotes that are alien to a currency using wave or particle radiation
    • G07D7/12—Visible light, infrared or ultraviolet radiation
    • G—PHYSICS
    • G07—CHECKING-DEVICES
    • G07D—HANDLING OF COINS OR VALUABLE PAPERS, e.g. TESTING, SORTING BY DENOMINATIONS, COUNTING, DISPENSING, CHANGING OR DEPOSITING
    • G07D7/00—Testing specially adapted to determine the identity or genuineness of valuable papers or for segregating those which are unacceptable, e.g. banknotes that are alien to a currency
    • G07D7/06—Testing specially adapted to determine the identity or genuineness of valuable papers or for segregating those which are unacceptable, e.g. banknotes that are alien to a currency using wave or particle radiation
    • G07D7/12—Visible light, infrared or ultraviolet radiation
    • G07D7/1205—Testing spectral properties
    • G—PHYSICS
    • G07—CHECKING-DEVICES
    • G07D—HANDLING OF COINS OR VALUABLE PAPERS, e.g. TESTING, SORTING BY DENOMINATIONS, COUNTING, DISPENSING, CHANGING OR DEPOSITING
    • G07D7/00—Testing specially adapted to determine the identity or genuineness of valuable papers or for segregating those which are unacceptable, e.g. banknotes that are alien to a currency
    • G07D7/20—Testing patterns thereon
    • G07D7/202—Testing patterns thereon using pattern matching
    • G07D7/205—Matching spectral properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M3/00—Printing processes to produce particular kinds of printed work, e.g. patterns
    • B41M3/14—Security printing
    • B41M3/144—Security printing using fluorescent, luminescent or iridescent effects
    • 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
    • G01N21/6456—Spatial resolved fluorescence measurements; Imaging

Definitions

  • the present invention relates to a device, systems and methods for semi- forensically detecting preconfigured patterns, colors and their combination and uses thereof. Specifically, the disclosure relates to a device adapted to selectively excite and detect emission of a preconfigured pattern of photoluminescence sources and their use for authenticating articles of manufacture.
  • Tagging has been requested by manufacturers, distributors and governments alike in order to mitigate the aforementioned issues. Tagging can be done by for example, adding a colorant, a fluorescent compound, or other easily detectable markers.
  • tagging technologies for plastics and polymers may cause adverse effects to the properties of the product, or may not be compatible with the production process of the plastic product due to challenging temperatures and pressures encountered in the production process.
  • the taggant materials may interfere with, or be affected by, the mixture of chemicals existing in the mixture.
  • fluorescent carbon-based materials relates to carbon materials having fluorescence properties (for the sake of brevity, the term “fluorescence” would be used herein also to refer interchangeably to photoluminescence (PL)) in the context of this description
  • fluorescent carbon-based materials encompass carbon molecules, carbon-based oligomers and polymer/co-polymer structures, carbon dots (CDs), photoluminescent carbon nanostructures (PCNs) such as graphene quantum dots (fluorescent carbon-based materials), graphene oxide quantum dots, carbon nanotube quantum dots or a combination of one or more of said materials.
  • the fluorescent carbon-based materials may originate from any organic carbon source which is non-toxic or otherwise not deleterious to the intended use.
  • the carbon nanotube quantum dots can be single wall nanotube (SWNT), or multi-wall nanotube (MWNT), or a combination thereof.
  • a hyperspectral/multispectral imaging system comprising: an illumination module configured to illuminate a subject; an optical acquisition module adapted to acquire photons emitted from the subject; a display a central processing module (CPM); a display in communication with the CPM; and a memory in communication with the CPM having thereon a processor-readable medium with a set of executable instructions configured to cause the CPM to: in response to activation by a user, illuminate the subject; detect photons emitted from the subject; and display a pattern represented by the emitted photons.
  • CPM central processing module
  • a method of authenticating an article of manufacture having thereon an area of interest (AOI) adapted to emit photons at a predetermined spectra, in a predetermined pattern, or their combination comprising: using a hyperspectral/multispectral imaging system, detecting the pattern and/or spectra of photons emitted by the AOI; comparing the detected pattern and/or spectra with a pattern and/or spectra associated with an authentic article of manufacture; and if the pattern and/or spectra detected is homologous to the pattern associated with the authentic article of manufacture, authenticating the article; otherwise providing an indication that the pattern detected is not homologous to the pattern associated with the authentic article of manufacture.
  • AOI area of interest
  • arranging the plurality of fluorescent carbon- based materials in the area of interest comprises the steps of:
  • an ink jet printing system comprising a first print head having at least one aperture, a first inkjet ink reservoir, and a pump configured to supply the first inkjet ink through the aperture;
  • a second print head having: at least one aperture, a second inkjet ink reservoir, and a pump configured to supply the second inkjet ink through the aperture; c) providing a conveyor, operably coupled to the first, and the second print heads configured to convey a substrate to each of the first, and second print heads; d) providing and a computer aided manufacturing (“CAM”) module, comprising a data processor, a non-volatile memory, and a set of executable instructions stored on the non-volatile memory for receiving a 2D visualization file representing predetermined pattern;
  • CAM computer aided manufacturing
  • the plurality of photoluminescent dots are arranged in a polymer substrate which is a thermoset polymer selected from: poly(epoxide), an acrylic, poly(dimethylsiloxane) thermoset, poly(urethanes), a copolymer thereof or their combination.
  • a thermoset polymer selected from: poly(epoxide), an acrylic, poly(dimethylsiloxane) thermoset, poly(urethanes), a copolymer thereof or their combination.
  • thermoplastic polymer selected from: Acrylonitrile butadiene styrene (ABS), poly(vinylchloride) (PVC), High density poly(ethylene) (HDPE), Low density poly(ethylene) (LDPE), Poly(propylene) (PP), poly(styrene) (PS), poly(methylmethacrylate) (PMMA), Natural rubber (NR), poly(oxymethylene) (POM), Polycarbonate (PC), Poly(ethylene terephthalate) (PET), poly(etheretherketone) (PEEK), poly(caprolactam) (Nylon 6, PA6), a copolymer thereof, terpolymer thereof, or their combination.
  • ABS Acrylonitrile butadiene styrene
  • PVC poly(vinylchloride)
  • HDPE High density poly(ethylene)
  • LDPE Low density poly(ethylene)
  • PP Poly(propylene)
  • PS poly(styrene)
  • PMMA poly(methylmethacrylate
  • the polymeric product is an identification item, and in other embodiments, the polymeric product is an ornamental item.
  • the polymeric product is manufactured by the steps of: adsorbing fluorescent carbon-based materials onto a carrier to form a carrier-fluorescent complex; mixing the carrier-fluorescent complex with a thermoset polymer resin, forming a master batch; optionally, diluting the master batch with thermoset polymer resin; and admixing the master batch with the thermoset hardener, thereby initiating curing.
  • the master batch is diluted with said thermoset polymer to a concentration of between 0.1-5 %wt.
  • the curing comprises crosslinking, photocuring, or a curing combination comprising the foregoing.
  • the method comprises a step of molding the process batch prior to curing.
  • mixing the carrier-fluorescent complex with the thermoset polymer resin is performed at a maximum loading level of between 20-30 %wt of carrier to resin, depending on the carrier and the resin.
  • the polymeric product is manufactured by the steps of: adsorbing fluorescent carbon-based materials onto a carrier to form a carrier-fluorescent complex; mixing the carrier-fluorescent complex with a composition comprising a thermoplastic polymer, under extrusion conditions, forming a master batch; and diluting the master batch with a thermoplastic resin, thereby forming a process batch ready for injection molding.
  • the extrusion conditions are at between 200°C -300°C and at loading level of 0.1-10 %wt of carrier to resin.
  • adsorbing fluorescent carbon-based materials onto a carrier comprises the steps of: solubilizing the fluorescent carbon-based materials in a solvent; adding the carrier to the fluorescent carbon-based materials solution under continuous mixing; separating the -fluorescent complex from the solvent; drying the carrier-fluorescent complex; and grinding the carrier-fluorescent complex into a fine powder.
  • adsorbing fluorescent carbon- based materials onto a carrier comprises the steps of: solubilizing the carrier in a solvent, optionally, under heating conditions; adding the fluorescent carbon-based materials to the carrier solution and mixing; drying the carrier-fluorescent complex; and grinding the carrier-fluorescent complex into a fine powder.
  • the solubilizing the carrier in a solvent is performed under heating conditions of between 60°C -80°C.
  • drying the carrier-fluorescent complex is done in a vacuum oven at a temperature of between 60°C -120°C and between 20-50 mBar.
  • the carrier in the above methods is an organic or inorganic micron sized material examples being - starch, AI203, Ti02, ZnO, Ce02, Si02, CaC03, or a combination thereof.
  • the ratio between the fluorescent carbon-based materials and the carrier is between 1:850 and 1:50, or between 100 ppm and 20,000 ppm.
  • the solvent is selected from: ethanol (EtOH), isopropyl alcohol (IPA), water, or a solvent composition comprising one or more of the foregoing.
  • the step of mixing the carrier- fluorescent complex is preceded by filtering the carrier-fluorescent complex.
  • the step of mixing the master batch with the thermoplastic resin is followed by a step of forming the process batch into pellets, rods, powder or a physical form comprising one or more of the foregoing.
  • the polymeric product is manufactured by impregnating a thermoplastic polymer with fluorescent carbon-based materials comprising the steps of: forming a powder comprising composite thermoplastic polymer and the fluorescent carbon-based materials; using a first solvent which is thermodynamically compatible with both the thermoplastic polymer and the fluorescent carbon-based materials, solubilizing the powder; and removing the first solvent forming a composite powder of thermoplastic polymer and fluorescent carbon-based materials.
  • the method further comprises washing the powder with a second solvent which may optionally be thermodynamically compatible with the fluorescent carbon-based materials only.
  • the second solvent is the same as the first solvent.
  • the second solvent is acetone.
  • the step of forming the composite powder of thermoplastic polymer and fluorescent carbon-based materials comprises the following steps: admixing the thermoplastic polymer into a reactor containing the first solvent, forming a polymer solution; while stirring, admixing the fluorescent carbon- based materials into the polymer solution forming composite thermoplastic polymer- fluorescent solution; transferring the composite thermoplastic polymer-fluorescent solution to a dryer; removing the first solvent, forming a coarse cake; and milling the coarse cake, forming a fine powder of composite thermoplastic polymer and fluorescent carbon-based materials.
  • the mill is a hammer mill or a ball mill.
  • the fluorescent carbon- based materials are modified to be thermodynamically compatible with the thermoplastic or thermoset polymer.
  • the polymeric product manufactured according to the above methods is an identification item. According to some other embodiments, the polymeric product manufactured according to the above methods, is an ornamental item.
  • FIG. 1 schematically illustrates a portable system according to one embodiment of the invention
  • Fig. 2 is a schematic illustration of a discrete illumination device, detector and optional filters disposed above the area of interest (AOI); and
  • FIG. 3 shows examples of preconfigured patterns of AOI's as detected by (from left to right), detector with increasing spectral resolution, at varying excitation wavelengths.
  • the disclosure relates to a device adapted to selectively excite and detect emission of a preconfigured pattern and/or spectra (e.g., color) of fluorescent carbon-based materials and their use for authenticating articles of manufacture.
  • spectra e.g., color
  • a and/or B can be used as either A alone, B alone or as A and B together.
  • preconfigured pattern and/or spectra (e.g., color) of carbon pattern indicating compounds refers to embodiments where the detectors are configured to detect only color of the photoluminescence sources, only the pattern created by the photoluminescence sources, or a combination of color AND pattern of the photoluminescence sources in the area of interest (AOI).
  • the articles of manufacture that can be tagged, identified and authenticated using the systems, devices, and methods described herein can be, for example, articles printed using additive manufacturing technologies, oriented circuit boards, food and pharmaceutical packaging, or other articles of manufacture where source identifying is important to ensure consumers, producers, distributors and government of the origin of the items thus tagged.
  • a system 10 comprising a device 100 with a detector configured to detect photonic emission from a substrate, as schematically illustrated in Fig. 1.
  • the device of Fig. 1 is provided with a detector, a power source and a plurality of excitation sources for emitting electromagnetic radiation (EMR), as further discussed herein below.
  • EMR electromagnetic radiation
  • the device can be configured to be handheld, and in the embodiment shown in the figure, it is powered by a smart phone 200, via cable 150, connected, in this particular example, via USB port 250.
  • the device can be connected wirelessly, e.g., via Bluetooth.
  • Device 100 can then recognize a specific substrate, schematically illustrated in the fig. by 300.
  • the plurality of excitation sources for emitting electromagnetic radiation (EMR) in the device and systems described herein can be adapted to emit EMR with narrow full width at half maximum (FWHM).
  • the electromagnetic radiation source can be a light emitting diode (LED) adapted to provide light at a discrete wavelength, a LASER source (e.g., a laser diode or diodes), or a light source coupled to appropriate optical filter.
  • a LASER source e.g., a laser diode or diodes
  • a light source coupled to appropriate optical filter As indicated, there can be more than one LED thus providing simultaneous excitation at various wavelengths, as there can be more than a single LASER source or light source with optical filters that limit the wavelength spectrum exciting the fluorescent carbon-based materials, for example, carbon polymer dots (CPDs).
  • CPDs carbon polymer dots
  • EMR emitting sources can be, for example, light emitting diodes (LEDs) configured to emit light at a very narrow wavelength without generating heat.
  • the LEDs can be configured to have a central wavelength (CWL) that coincides with the peak excitation wavelength of fluorescent carbon-based materials forming the pattern or configured to provide a particular color combination (spectra), while the full width at half maximum (FWHM) can be configured to be narrow enough so as not to substantially overlap with the excitation wavelength of other fluorescent carbon-based materials forming the pattern and/or the desired spectra.
  • CWL central wavelength
  • FWHM of the EMR sources can be between 10 nm and 20 nm.
  • the FWHM of the photoluminescence sources (PCNs) can be configured to be between 30-40 nm.
  • Fig. 2 schematically illustrates the setup of device 100.
  • 120 is an actuating button
  • 130 is an optical future that can be switched between different filters
  • 110 indicates one or more excitation sources
  • 300 is the base of device 100
  • 350 schematically illustrates samples being analyzed by device 100.
  • the detector can be used to detect only color emitted from fluorescent carbon sources imbedded homogenously in a polymer or print matrix.
  • the detector can be configured to resolve emitting fluorescent carbon sources features loaded onto an inorganic filler in the size between about 2 pm and about 1000 pm, dispersed heterogeneously in a polymer matrix (in other words, the spatial resolution requirement).
  • fluorescent carbon-based materials dispersed in pure form or adsorbed on an inorganic filler, it is possible to achieve the effect of photoluminescence in the AOI completely without any effect on the properties of the matrix.
  • fluorescent carbon-based materials such as, for example, carbon polymer dots (CPDs)
  • CPDs carbon polymer dots
  • nanometric or sub-nanometric materials e.g., between about 0.2 nm and up to 25 nm. Therefore, when embedded in the polymer in pure form, their size is under the light diffraction limit and they are invisible to the naked eye while still fluorescing throughout the bulk of the matrix.
  • size reduction techniques can be used to produce fine sub-micron particles that are homogenously dispersed in the matrix and maintain their photoluminescence.
  • inorganic fluorescent pigments which may also be used in such applications, and which will almost always have some effect on the optical properties of the matrix they are blended into.
  • the size of these pigments cannot be reduced without limit as their photoluminescence depends on their crystal structure which accumulates defects as the size reduces.
  • the fluorescent carbon-based materials used in the compositions, devices and methods provided herein are stable at high temperatures, high pressure and shear force, show relative inertness to changing chemical environments and are usually more photostable than organic dyes which may perform similarly in terms of initial Quantum Yield (QY), they improve the durability of the marking.
  • QY Quantum Yield
  • This, in combination with their high QY enables their loading into polymeric and ink mixtures in ultra-low levels (e.g., about 10 ppm in various systems, or about lppm in bulk liquids) while retaining significant fluorescence.
  • "low loading” will depend on the pigmentation of the material tagged/authenticated.
  • a loading of, for example loading of 0.01% (w/w) will be considered low loading in non- or sparsely pigmented items, while 0.1% (w/w) (or between about 100 ppm and about 1000 ppm) may be considered as low loading for pigmented items or systems.
  • This low loading can be advantageous when compared with the loading levels required for other organic or inorganic dyes with requiring loading levels of 0.2% and more up to 5% (w/w).
  • Fig. 3 illustrates the different levels of detection that can be achieved by inspecting a tagged item. Looking at the 365 nm range, level 1 detector level 2 detector and level 3 detector provide very different levels of detection. The different Ivels represent different spatial and spectral resolutions. For example, level 2 has a greater spatial resolution than level 1, and level 3 has a greater spectral resolution. Moreover, Fig. 3 only shows two states (A and B), but of course other states can be used, at different wavelength, and a scanning procedure may involve a plurality of such states. The colors in this fig.
  • identifying patterns can be generated such that when read in a specific sequence using different level detectors, a clear identification of a tagged product can be achieved.
  • system as used herein shall also be taken to include any collection of systems or sub-systems that individually or jointly execute a set, or multiple sets, of instructions to perform one or more functions. Also, the term “system” refers to a logical assembly arrangement of multiple devices, and is not restricted to an arrangement wherein all of the component devices are in the same housing.
  • a hyperspectral/multispectral imaging system comprising: an illumination module configured to illuminate a subject using a plurality of discrete wavelengths in a predetermined sequence; an optical acquisition module adapted to acquire photons emitted from the subject; a display; a central processing module (CPM); a display in communication with the CPM; and a memory in communication with the CPM having thereon a processor-readable medium with a set of executable instructions configured to: in response to activation by a user, illuminate the subject; detect photons emitted from the subject; and display a pattern represented by the emitted photons.
  • an illumination module configured to illuminate a subject using a plurality of discrete wavelengths in a predetermined sequence
  • an optical acquisition module adapted to acquire photons emitted from the subject
  • a display a central processing module (CPM); a display in communication with the CPM; and a memory in communication with the CPM having thereon a processor-readable medium with a set of executable instructions configured to: in response to
  • the system and devices disclosed herein can be adapted to perform hyperspectral and/or multispectral imaging, referring to methods and devices for acquiring hyperspectral and/or multispectral data sets or data-cubes, which typically comprise images where continuously sampled, finely resolved spectral information is provided at each pixel (see e.g., Fig. 3).
  • the imaging device 100 of Fig. l may be a multi-spectral imaging device having a plurality of sensors 120 (as shown in Fig. 2) for collecting spectra (and thus intensity) data in a plurality of different wavelengths, for example 3 to 10 in number (see e.g., Fig. 3), from the predetermined fluorescent carbon-based pattern in the AOI.
  • multi-spectral imaging device 100 may be configured to collect spectra data in 4 or more different wavelengths, or 6 or more different wavelengths.
  • 'module' means, but is not limited to, a software and/or hardware component, such as a Field Programmable Gate-Array (FPGA) or Application-Specific Integrated Circuit (ASIC), which performs certain tasks.
  • a module may advantageously be configured to reside on the addressable storage medium and configured to execute on one or more processors.
  • a module may include, by way of example, components, such as software components, object-oriented software components, class components and task components, processes, functions, attributes, procedures, subroutines, segments of program code, drivers, firmware, microcode, circuitry, data, databases, data structures, tables, arrays, and variables.
  • components such as software components, object-oriented software components, class components and task components, processes, functions, attributes, procedures, subroutines, segments of program code, drivers, firmware, microcode, circuitry, data, databases, data structures, tables, arrays, and variables.
  • the functionality provided for in the components and modules may be combined into fewer components and modules or further separated into additional components and modules.
  • the illumination module used in the devices and systems described herein, implemented in the methods described can comprise a plurality of electromagnetic radiation emitters configured to emit radiation at a predetermined wavelength range.
  • the plurality e.g., one EMR emitter per fluorescent carbon-based materials.
  • EMR emitters can be LEDs with discrete central wavelength (CWL), for example, as illustrated in Fig.
  • the plurality of EMR emitters can be configured to illuminate the sample discretely (in other words, one at a time), in a preconfigured sequence.
  • illumination of a first AOI can have the sequence Green:Cyan:Orange; while illumination of a second AOI can have the sequence Purple:Cyan:Green.
  • the response in each illumination sequence can then be recorded and form a part of the authentication procedure.
  • the optical acquisition module comprises a detection element that is a photodetector, a charge-coupled device (CCD), diode array, complimentary metal-oxide sensor device (CMOS), a focal plane array or a detection element comprising one or more of the foregoing.
  • the optical acquisition module is configured generally to parse received image into multiple distinct classes based on which axes of the data-cube (portion or all the AOI) are sampled at a given instant.
  • the optical acquisition module can instantaneously sample the pattern along the spectral axis (e.g., from about 190 nm to about 720 nm) and along one spatial axis (see e.g., top row, Fig. 3 level 2 detector), but the other spatial axis must be scanned in time to build up a full data-cube.
  • light that impinges on an entrance slit can be dispersed through a grating or a prism, and the dispersed light is imaged onto a two-dimensional detector array.
  • the full datacube is built up and displayed using the device/system display (see e.g., 200, Fig. 1).
  • IR Infrared
  • NIR near infrared
  • IR and NIR spectroscopies generally involves the absorption of radiation as it passes through a sample. The absorption frequencies can therefore provide information regarding the chemical and physical characteristics or the molecular structure of the irradiated substance and its composition.
  • the CPM is in electronic communication with a library comprising the hyperspectral and/or multispectral patterns.
  • the library can serve as reference for the pattern detected and can include expected emission spectra at each wavelength as a function of the spatial resolution used in the AOI.
  • the set of executable instructions are further configured to cause the CPM to analyze the detected pattern, and to provide a comparison between the detected pattern and the pattern obtained from the library. The comparison can then be used to authenticate the article of manufacture as identical to the source, or as a fake if the degree of homology (in other words, identity) is below a certain threshold, for example, less than 95%, or less than 90%, or in circumstances where the article has been subjected to intensive wear and tear, even less.
  • the subject of the analysis is a substrate forming a portion of the article of manufacture, which can either be exposed to the environment, or otherwise concealed.
  • the subject can be a substrate comprising an area of interest (AOI) adapted to emit photons at a predetermined spectrum in a predetermined pattern, wherein the predetermined pattern is the pattern displayed.
  • AOI area of interest
  • the pattern can comprise a plurality of fluorescent carbon-based materials arranged in an embodiment as an array of unique combination (that can be stored in the library).
  • the area of interest can be comprised of a plurality of fluorescent carbon-based materials arranged in a two-dimensional formation adapted to produce the predetermined pattern.
  • That pattern is then recognized by the device and compared with the pattern stored in the linked library, whereupon either the final authentication determination is provided, or the detected pattern and the stored pattern are compared by either overlaying or by rendering the patterns on the display - side-by-side.
  • the pattern can have dimensions that are less than half the wavelength of visible light, thus making the pattern invisible to the naked eye.
  • the output of the detection device can vary from providing the average value of chroma (the strength of the surface color), hue (the dominant wavelength mode) and lightness of the whole sample (AOI), as well as degree of saturation when discretely illuminated at each wavelength provided by the plurality of EMR emitters. These values can then be compared with stored values of an authentic sample and be used to verify the source of the sample. Also, the detecting device can be configured to recognize 2D spatial arrangements of patterns and compare those with stored patterns. Moreover, when hyperspectral imaging is used in the detection, the actual emission spectral bands can be used.
  • Embodiments described herein may comprise or utilize a special purpose or general-purpose computer including computer hardware, such as, for example, one or more processors (e.g., central processing module, CPM) and system memory, as discussed in greater detail below.
  • Embodiments described herein also include physical and other computer-readable media for carrying or storing computer-executable instructions and/or data structures.
  • Such computer-readable media can be any available media that can be accessed by a general purpose or special purpose computer system.
  • Computer-readable media that store computer-executable instructions are physical storage media.
  • Computer-readable media that carry computer-executable instructions are transmission media.
  • embodiments of the invention can comprise at least two distinctly different kinds of computer-readable media: computer storage media and transmission media.
  • Forming the pattern can be done in an embodiment, using inkjet printing, as indicated, by creating minimally loaded inkjet inks having the fluorescent carbon-based materials dispersed therein, capable of emitting photons in response to excitation at discrete wavelengths.
  • arranging the plurality of fluorescent carbon-based materials in the two-dimensional formation thus forming the predetermined pattern detected by the devices and systems provided can comprises: providing an inkjet printing system comprising: a first print head having: at least one aperture, a firs inkjet ink reservoir, and a pump configured to supply the first inkjet ink through the aperture; a second print head having: at least one aperture, a second inkjet ink reservoir, and a pump configured to supply the second inkjet ink through the aperture; a conveyor, operably coupled to the first, and the second print heads configured to convey a substrate to each of the first, and second print heads; and a computer aided manufacturing (“CAM") module, comprising: a data processor; a non-volatile memory; and a set of executable instructions stored on the non-volatile memory for: receiving a 2D visualization file representing predetermined pattern; generating a file that represents the predetermined pattern for printing; receiving a selection of parameters related to the area of interest;
  • CAM computer aide
  • the fluorescent carbon-based materials can be nano-sized (of less than 10 nm in size) structures of carbon molecules (more than a single atom) having dimensionality that is anywhere from quasi-one dimension (e.g., quantum dot, nanoribbon, nanobelt), to three dimensional (e.g., multilayer graphene structures).
  • quasi-one dimension e.g., quantum dot, nanoribbon, nanobelt
  • three dimensional e.g., multilayer graphene structures
  • the polymeric products are characterized as having uniform fluorescence. While in other embodiments, the polymeric products have a patterned fluorescence.
  • the polymeric products may also comprise fluorescent carbon- based materials having different emission wavelengths producing different colors under electromagnetic radiation (EMR). Polymeric products having unique patterning can be used in authentication and tagging of products. Thus, in some embodiments, the polymeric product is an identification item.
  • polymeric product of the invention may have a more aesthetic or decorative value.
  • the polymeric product is an ornamental item.
  • Detecting which in another embodiment also includes quantifying emission spectra, can be done, by detecting luminescence of the measured pattern.
  • Luminescence spectroscopy involves the measurement of photon emission from molecules. It can include photoluminescence such as fluorescence and phosphorescence, which are emissions from a substance resulting from its excitation by radiation absorption, as well as chemiluminescence, where the emission is induced by a chemical reaction.
  • the emitted radiation is characteristic of the molecular structure, size and composition. Accordingly, manipulating the structure, size and composition of both the fluorescent carbon-based materials (interchangeable with CQDs), as well as the inkjet ink composition, it is possible to fabricate an AOI having a detectable, repeatable pattern.
  • a photodetector array e.g., a PIN diode array
  • different color filters and EMR sources based on the plurality of CQDs used in the pattern, as well as provide an UV/VIS/NIR bandpass(es) color filter(s) operably coupled to a photodetector array.
  • a (scanning) diffraction grating coupled to a photodetector array can be used to determine the spectrum profile emitted from the plurality of CQDs.
  • Detection can be quantified, yielding peak emission, half peak baseline, intensity and area under the curve (AUC), as well as ratios of the foregoing, as a function of excitation wavelength (see e.g., Fig 3); all which can be added to the linked library database at the device or system and used to compare with the test sample obtained by an end user or intermediate downstream (pipeline or supply chain).
  • the control over peak emission spectra of the photoluminescence sources is not necessarily solely a function of size, but of other factors as well, for example; the type of photoluminescence sources (e.g., fluorescent carbon- based materials, lanthanide nanorod, or MWCNT) the extent and location of surface defects in the fluorescent carbon-based materials when used, type and degree of substitution of various functional groups (e.g., carboxylate) as well as uniformity of size distribution and other factors. Accordingly, it is contemplated that fluorescent carbon- based materials having exactly the same overall average D3,2 particle size (e.g., ⁇ 5.0 nm), would nevertheless have peak emission spectra that is shifted between about 20 nm and about 80 nm.
  • the type of photoluminescence sources e.g., fluorescent carbon- based materials, lanthanide nanorod, or MWCNT
  • various functional groups e.g., carboxylate
  • EMR electromagnetic radiation
  • a handheld device housing having: a display; a processing module comprising a processor in communication with a linked library containing original pattern emission spectra at a specific wavelength, of the carbon quantum dot formed on the pattern in the AOI on the article of manufacture sought to be identified and/or authenticated; the processor further being in communication with: the plurality of electromagnetic radiation sources; a detector (e.g., a photodetector) configured to detect fluorescence, phosphorescence, chemiluminescence or their combination (and can further comprise additional optical color filters); the display; and a non-volatile memory having thereon a processor-readable medium with a set of executable instructions configured to: receive a reading from the detector; retrieve from the linked library a predetermined: emission spectra; and if the detected pattern emission spectra at a specific wavelength, retrieved from the detector correlates with the pattern emission spectra, at the predetermined specific wavelength, wavelength range or wavelength range
  • a method of authenticating an article of manufacture having thereon an area of interest (AOI) adapted to emit photons at a predetermined spectra, in a predetermined pattern and/or spectra comprising: using a hyperspectral/multispectral imaging system, detecting the pattern and/or spectra (color) of photons emitted by the photons in response to exposure to a plurality of discrete EMR sourced emitting discrete wavelength at a predetermined sequence (wherein the discrete wavelength is between about 200 and 500 nm); comparing the detected pattern and/or spectra with a pattern associated with an authentic article of manufacture; and if the pattern and/or spectra detected is homologous to the pattern and/or spectra associated with the authentic article of manufacture, authenticating the article; otherwise providing an indication that the pattern and/or spectra detected are not homologous to the pattern associated with the authentic article of manufacture
  • the methods using the PCNs' patterns disclosed and claimed herein, implemented using the devices and systems described herein can further comprise comparing the detected emission pattern and/or spectra to a predetermined pattern and/or spectra corresponding to an authentic identity; and if the detected spectra correlates with the predetermined emission pattern and/or spectra, authenticating the article; else identifying the article as non-authentic.
  • authentic means that the pattern and/or spectra detected by the device has high correlation with the emission pattern and/or spectra obtained at the original source.
  • the housing comprising the plurality of EMR sources (configured to emit EMR at discrete wavelength range of between NMT about 500 nm, or below full visible wavelength range), can further comprise a transceiver configured to initiate communication with remote computing systems.
  • the EMR source is an actinic radiation source, configured to produce photochemical reaction in the pattern disposed on the substrate.
  • each EMR source can be configured to emit electromagnetic radiation at a wavelength between about 0.8 nm (laser equipped with power stabilizer) and about 450 nm, or between about 160 nm and about 300 nm, for example, between 190 nm and 250 nm.
  • processors of the associated computing system(s) that performs the act direct the operation of the computing system in response to having executed computer-executable instructions.
  • An example of such an operation involves the manipulation of data.
  • the computer- executable instructions (and the manipulated data) may be stored in the memory of the computing system.
  • Computing system may also contain communication channels that allow the computing system to communicate with other processors and sensors over, for example, service bus.
  • Embodiments described herein may comprise or utilize a special purpose or general-purpose computer including computer hardware, such as, for example, one or more processors (e.g., central processing module, CPM) and system memory, as discussed in greater detail below.
  • Embodiments described herein also include physical and other computer-readable media for carrying or storing computer-executable instructions and/or data structures.
  • Such computer-readable media can be any available media that can be accessed by a general purpose or special purpose computer system.
  • Computer-readable media that store computer-executable instructions are physical storage media.
  • Computer-readable media that carry computer-executable instructions are transmission media.
  • embodiments of the invention can comprise at least two distinctly different kinds of computer-readable media: computer storage media and transmission media.
  • Computer storage media includes RAM, ROM, EEPROM, CD-ROM or other optical disk storage, magnetic disk storage or other magnetic storage devices, or any other medium which can be used to store desired program code means in the form of computer-executable instructions or data structures and which can be accessed by a general purpose or special purpose computer.
  • module is used herein to refer to software computer program code and/or any hardware or circuitry utilized to provide the functionality attributed to the module. Further, the term “module” or “component” can also refer to software objects or routines that execute on the computing system. The different components, modules, engines, and services described herein may be implemented as objects or processes that execute on the computing system (e.g., as separate threads).
  • the CPM may be operably coupled to the various modules and components with appropriate circuitry may also be used herein, the term(s) "operably coupled to", “coupled to”, and/or “coupling” includes direct coupling between items and/or indirect coupling between items via an intervening item (e.g., an item includes, but is not limited to, a component, an element, a circuit, an engine, and/or a module) where, for indirect coupling, the intervening item does not modify the information of a signal but may adjust its current level, voltage level, and/or power level.
  • an intervening item e.g., an item includes, but is not limited to, a component, an element, a circuit, an engine, and/or a module
  • the intervening item does not modify the information of a signal but may adjust its current level, voltage level, and/or power level.
  • inferred coupling includes direct and indirect coupling between two items in the same manner as “coupled to”.
  • operble to or “operably coupled to” indicates that an item includes one or more of power connections, input(s), output(s), etc., to perform, when activated, one or more its corresponding functions and may further include inferred coupling to one or more other items.
  • associated with includes direct and/or indirect coupling of separate items and/or one item being embedded within another item.
  • central processing module may be a single processing device or a plurality of processing devices.
  • a processing device may be a microprocessor, micro-controller, digital signal processor, microcomputer, central processing unit, field programmable gate array, programmable logic device, state machine, logic circuitry, analog circuitry, digital circuitry, and/or any device that manipulates signals (analog and/or digital) based on hard coding of the circuitry and/or operational instructions.
  • the processing module, processing circuit, and/or processing unit may have an associated memory and/or an integrated memory element, which may be a single memory device, a plurality of memory devices, and/or embedded circuitry of the processing module, module, processing circuit, and/or processing unit.
  • a memory device may be a read-only memory, random access memory, volatile memory, non-volatile memory, static memory, dynamic memory, flash memory, cache memory, and/or any device that stores digital information.
  • processing module, module, processing circuit, and/or processing unit includes more than one processing device, the processing devices may be centrally located (e.g., directly coupled together via a wired and/or wireless bus structure) or may be distributed (e.g., cloud computing via indirect coupling via a local area network and/or a wide area network). Further note that if the processing module, module, processing circuit, and/or processing unit implements one or more of its functions via a state machine, analog circuitry, digital circuitry, and/or logic circuitry, the memory and/or memory element storing the corresponding operational instructions may be embedded within, or external to, the circuitry comprising the state machine, analog circuitry, digital circuitry, and/or logic circuitry.
  • the memory element may store, and the processing module, module, processing circuit, and/or processing unit executes, hard coded and/or operational instructions corresponding to at least some of the steps and/or functions illustrated in one or more of the figures.
  • Such a memory device or memory element can be included in an article of manufacture.
  • the terms "a”, “an” and “the” herein do not denote a limitation of quantity, and are to be construed to cover both the singular and the plural, unless otherwise indicated herein or clearly contradicted by context.
  • the suffix "(s)” as used herein is intended to include both the singular and the plural of the term that it modifies, thereby including one or more of that term (e.g., the network(s) includes one or more network).
  • system shall also be taken to include any collection of systems or sub-systems that individually or jointly execute a set, or multiple sets, of instructions to perform one or more functions. Also, the term “system” refers to a logical assembly arrangement of multiple devices, and is not restricted to an arrangement wherein all of the component devices are in the same housing.
  • the sample is excited with light in different wavelengths (365nm, 395nm, 420nm) and the emission and color response, resulting from the combination of the fluorescent carbon materials with the polymer and possibly a pigment, yields a different value in the color space for each wavelength.
  • the resulting values are compared with a pre-stored reference sample to determine the authenticity of the article.
  • the sample is excited with light in different wavelengths (365nm, 395nm, 420nm) and the emission and color response, resulting from the combination of the fluorescent carbon materials with the polymer and possibly a pigment, yields a different value in the color space for each wavelength.
  • the resulting values are compared with a pre-stored reference sample to determine the authenticity of the article.
  • the sample is excited with light in different wavelengths (365nm, 395nm, 420nm) and the emission and color response, resulting from the combination of the fluorescent carbon materials with the polymer and possibly a pigment, yields a different value in the color space for each wavelength.
  • the resulting values are compared with a pre-stored reference sample to determine the authenticity of the article.
  • the emitting micron sized carriers can be also spatially resolved and analyzed for their proportion in the total population as well as for their size and other shape parameters (such as curvature, X/Y/Z proportion etc.)
  • the sample is excited with light in different wavelengths (365nm, 395nm, 420nm) and the emission and color response, resulting from the combination of the fluorescent carbon materials with the polymer and possibly a pigment, yields a different spectral emission pattern for each of the different fluorescent carbon materials present in the sample.
  • the resulting parameters are then compared with a pre-stored reference sample to determine the authenticity of the article:
  • the emitting micron sized carriers are spatially resolved and analyzed for their proportion in the total population as well as for their size and other shape parameters (such as curvature, X/Y/Z proportion etc.)

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Abstract

L'invention concerne un dispositif, des systèmes et des procédés de détection d'un motif préconfiguré et/ou de spectres et leurs utilisations. Selon un aspect, l'invention concerne un dispositif conçu pour exciter et détecter sélectivement une émission photonique d'un motif préconfiguré et/ou de spectres de sources de photoluminescence et son utilisation, conjointement avec des matériaux de marquage appropriés, pour authentifier des articles manufacturés.
PCT/IL2019/050179 2018-02-16 2019-02-14 Lecteur de motif et/ou de spectres et ses utilisations WO2019159171A1 (fr)

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CN112058213A (zh) * 2020-09-18 2020-12-11 昆明理工大学 一种吸附废水中重金属Cr（Ⅵ）的方法
WO2024072344A1 (fr) * 2022-10-01 2024-04-04 Nanografi̇ Nano Teknoloji̇ Anoni̇m Şi̇rketi̇ Procédé de marquage pour le criblage dans différents spectres

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