WO2008127409A2 - Absorbeur d'infrarouge - Google Patents

Absorbeur d'infrarouge Download PDF

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Publication number
WO2008127409A2
WO2008127409A2 PCT/US2007/083779 US2007083779W WO2008127409A2 WO 2008127409 A2 WO2008127409 A2 WO 2008127409A2 US 2007083779 W US2007083779 W US 2007083779W WO 2008127409 A2 WO2008127409 A2 WO 2008127409A2
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WO
WIPO (PCT)
Prior art keywords
tin oxide
antimony tin
oxide nanoparticles
nanoparticles
antimony
Prior art date
Application number
PCT/US2007/083779
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English (en)
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WO2008127409A3 (fr
Inventor
Gregory T. Gaudet
Richard T. Zvosec
Mark Still
Valerie Russell
Original Assignee
Ppg Industries Ohio, Inc.
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.)
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Publication date
Application filed by Ppg Industries Ohio, Inc. filed Critical Ppg Industries Ohio, Inc.
Publication of WO2008127409A2 publication Critical patent/WO2008127409A2/fr
Publication of WO2008127409A3 publication Critical patent/WO2008127409A3/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G30/00—Compounds of antimony
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G19/00—Compounds of tin
    • C01G19/02—Oxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2949/00—Indexing scheme relating to blow-moulding
    • B29C2949/07—Preforms or parisons characterised by their configuration
    • B29C2949/0715—Preforms or parisons characterised by their configuration the preform having one end closed
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C49/00—Blow-moulding, i.e. blowing a preform or parison to a desired shape within a mould; Apparatus therefor
    • B29C49/0005—Blow-moulding, i.e. blowing a preform or parison to a desired shape within a mould; Apparatus therefor characterised by the material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C49/00—Blow-moulding, i.e. blowing a preform or parison to a desired shape within a mould; Apparatus therefor
    • B29C49/0005—Blow-moulding, i.e. blowing a preform or parison to a desired shape within a mould; Apparatus therefor characterised by the material
    • B29C49/0006—Blow-moulding, i.e. blowing a preform or parison to a desired shape within a mould; Apparatus therefor characterised by the material for heating or cooling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C49/00—Blow-moulding, i.e. blowing a preform or parison to a desired shape within a mould; Apparatus therefor
    • B29C49/02—Combined blow-moulding and manufacture of the preform or the parison
    • B29C49/06—Injection blow-moulding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2067/00—Use of polyesters or derivatives thereof, as moulding material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
    • B29K2105/06—Condition, form or state of moulded material or of the material to be shaped containing reinforcements, fillers or inserts
    • B29K2105/16—Fillers
    • B29K2105/162—Nanoparticles
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/51—Particles with a specific particle size distribution
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

Definitions

  • this invention relates to an antimony tin oxide (ATO) nanoparticle useful for infrared energy transfer. More specifically, in some embodiments, this invention relates to an ATO nanoparticle having a combination of particle size and particle composition that make it possible to achieve both high absorption of near infrared light and low absorption of visible light. In some embodiments, this invention relates to an ATO nanoparticle having a ratio of infrared absorbance to visible absorbance. In some embodiments, this invention also relates to composite materials, including, for example, polymers, inks and coatings, containing the ATO nanoparticle.
  • ATO antimony tin oxide
  • this invention also relates to using the ATO nanoparticle for energy transfer to a composite material, including infrared heating, curing or drying.
  • the present invention relates to an infrared absorber containing the ATO nanoparticle, and in some embodiments, the infrared absorber is capable of transferring energy to a medium suitable for supporting the infrared absorber, and in some embodiments, the medium is a polymer as well as uses and methods of making infra red absorber, compositions, and articles thereof.
  • PET poly(ethylene terephthalate)
  • OPP oriented polypropylene
  • a preform or parison is heated to a certain temperature and then blown to fill a mold.
  • the time required for the parison to reach the certain temperature is known as the reheat time or reheat rate of the material and varies as a function of the absorption characteristics of the polymer itself as well as any additives such as metals, catalysts, toners, dyes, or included foreign matter. With time, it has become possible to produce more bottles per hour, but it is still desirable to provide polymers which reheat faster or with less energy.
  • the heat lamps used in the beverage bottle industry typically are quartz lamps having a broad emission spectrum ranging from 500 nm to greater than 1500 nm. The quartz lamps' emission maximum is around 1100-1200 nm typically.
  • films such as PET and glass laminating adhesives such as poly (vinyl butyral) (PVB) are often treated with reflectors and/or absorbers to control the specific types of light that will pass through a window. This serves to reduce glare, deterioration of upholstery and carpeting, and heat entering a room or vehicle, among other things.
  • PVB poly (vinyl butyral)
  • reflectors and/or absorbers to control the specific types of light that will pass through a window.
  • reflectors and/or absorbers to control the specific types of light that will pass through a window.
  • reflectors and/or absorbers to control the specific types of light that will pass through a window.
  • reflectors and/or absorbers to control the specific types of light that will pass through a window.
  • reflectors and/or absorbers to control the specific types of light that will pass through a window.
  • reflectors and/or absorbers to control the specific types of light that will pass through a window.
  • nanoparticles of these materials have been used to make visibly transparent nanocomposite polymers and coatings with IR absorbing properties.
  • antimony tin oxide ATO is one of the less expensive of these materials, but unfortunately ATO is also one of the poorer performing materials in IR absorbing applications.
  • Antimony tin oxide is one of the transparent conductive oxides that has been used in thin film coatings.
  • Shanthi et. al. examined the optical and electrical properties of antimony tin oxide thin films, and they concluded that the optimum antimony content is 9%. (Crystal Res. Technol. Vol. 34, No. 8, pg. 1037- 1046 [1999]).
  • Antimony tin oxide has also been used in nanoparticle form as an additive for polymers, inks, and coatings.
  • the additive is intended to be used with an Nd:YAG laser that emits in the infrared at 1064 nm (Col. 3, Line 37).
  • Preferred ranges for antimony content are up to 17% (Col. 4, Line 25), but most preferably about 2% (Col. 4, Line 30).
  • Preferred ranges for particle size are between 10 and 70 nm, and more preferably between 20 and 50 nm (Col. 4, Line 29).
  • U.S. Patent Application Publication No. 2006-0269739 assigned to E I du Pont de Nemours and Company, discloses nanoparticulate solar control composites, which can be include nanoparticulate antimony tin oxide (Claim 1).
  • the preferred antimony content is 0.1 to 20 weight percent, more preferred 5 to 15 weight percent, still more preferred 8 to 10 weight percent (Paragraph 31).
  • the preferred particle size is less than 100 nm, with more preferred size less than 50 nm, still more preferred less than 30 nm, and still more preferred between about 1 nm and 20 nm (Paragraph 29).
  • the application shows that the antimony tin oxide is not optimized for the balance of infrared absorption and visible transparency, compared to the tin-doped indium oxide.
  • International Patent Application PCT/EP2003/007796 assigned to Merck Patent GMBH, discloses particulate semiconductor materials as a hardening or drying additive or for improving the thermal conductivity of lacquer systems and printing inks.
  • the particulate materials include mixtures of antimony oxide and tin oxide (Claim 5).
  • the particle sizes are between 10 nm and 2000 microns, preferably between 100 nm and 100 microns, more preferably between 500 nm and 30 microns.
  • the preferred dopant level is not disclosed specifically for antimony tin oxide, but for the semiconductor materials in general, the suitable level is disclosed as 0.01 to 30%, especially 5-16%.
  • the prior art for antimony tin oxide nanoparticles does not disclose a combination of particle size and particle composition that gives improved infrared absorbance.
  • the most preferred antimony composition in the prior art is generally between 5% and 16%, more specifically between 8% and 10%.
  • the prior art does not disclose an antimony tin oxide nanoparticle with a preferred particle size and particle composition to give a high ratio of infrared absorption to visible absorption.
  • This prior art is confirmed by commercially available antimony tin oxide nanoparticles (reference NanoPhase, American Elements, Inframat webpages, last checked March 2007), which have antimony content of 8%-10%, and particle size of between 10 nm and 30 nm.
  • a primary object of the invention to develop an ATO nanoparticle that makes it possible to achieve improved IR absorbing properties, suitable for transparent nanocomposites. This is achieved, in some embodiments, by making ATO having a particular combination of particle size distribution and particle composition.
  • ATO having a particular combination of particle size distribution and particle composition.
  • efforts to increase the IR absorption of coatings, inks, and adhesives are met with a number of problems, because the addition of IR absorbing material can adversely affect the performance and characteristics of the coatings, inks, or adhesives. For example, the IR absorbing material may alter the color or transparency of a coating, which is particularly problematic in applications such as clearcoats and color finishes.
  • the coatings, inks, or adhesives also may not absorb IR radiation uniformly depending on the distribution of the IR absorbing material in the coatings, inks, or adhesives.
  • the IR absorbing material may also adversely affect the performance of the coatings, such as be decreasing adhesivity of adhesives or making coatings less durable.
  • the present invention provides infrared (IR) absorbing nanoparticles that are substantially transparent to light in the visible spectrum.
  • IR infrared
  • the present invention also makes it possible to provide coatings, inks, and adhesives comprising these IR absorbing nanoparticles, and methods of drying and curing coatings, inks, and adhesives using IR energy.
  • FIG. 1 is a graph showing the absorbance of ethylene glycol comprising different IR absorbing materials as a function of wavelength. The graph demonstrates that nanoparticles of reduced indium tin oxide (rITO) and antimony tin oxide (New
  • Carbon black absorbs energy in both the IR and visible spectrums.
  • nanoparticles As used herein, “nanoparticles,” “nanoscale powders,” “nanocrystals,” and
  • Nanoparticles means particles with a mean diameter of less than 10 microns and an aspect ratio ranging from 1 to
  • the nanoparticles have a mean diameter of less than or equal to 250 nm. More embodiments are described below. In some embodiments, the nanoparticles have an aspect ratio ranging from 1 to 100. For example, a nanoparticle can have a mean diameter of 250 nm and an aspect ratio of
  • the invention is antimony tin oxide (ATO) nanoparticles having a mean particle size less than or equal to 250 nm and an antimony content greater than or equal to 5.0 atomic percent of the antimony tin oxide nanoparticles themselves.
  • ATO antimony tin oxide
  • the atomic percent of the antimony in the ATO nanoparticles may vary as explained here.
  • the antimony content is greater than or equal to 10.0 atomic percent of the antimony tin oxide nanoparticles themselves.
  • the antimony content is greater than or equal to 12.5 atomic percent of the antimony tin oxide nanoparticles themselves.
  • the antimony content is greater than or equal to 15.0 atomic percent of the antimony tin oxide nanoparticles themselves.
  • the antimony content is greater than or equal to 17.5 atomic percent of the antimony tin oxide nanoparticles themselves.
  • the antimony content is greater than or equal to 20.0 atomic percent of the antimony tin oxide nanoparticles themselves.
  • the antimony content ranges from 5.0 to
  • the antimony content ranges from 10.0 to 25.0 or 15.0 to 20.0 atomic percent of the ATO.
  • the figure of merit of the ATO nanoparticles may vary as explained here.
  • a figure of merit is be defined by the extinction of the composite material at 1100 nm ( ⁇ oonm) divided by the extinction at 550 nm ( ⁇ ssonm):
  • the FOM may be determined by a ratio of ODs:
  • the spectrophotometer should be set to receive a 2 nm band pass.
  • a higher FOM means that the nanocomposite does a better job of absorbing infrared light at 1100 nm while remaining transparent to visible light at 550 nm.
  • the FOM is strongly affected by both the particle size and particle composition, although the FOM is not strongly affected by the nanoparticle loading in the nanocomposite.
  • the antimony tin oxide nanoparticles which, when dispersed at 0.05 wt% (500 ppm) in ethylene glycol, have a figure of merit greater than or equal to 0.50.
  • the FOM is greater than or equal to 0.75. In some embodiments, the FOM is greater than or equal to 1.0. In some embodiments, the FOM is greater than or equal to 1.25. In some embodiments, the FOM is greater than or equal to 1.5. In some embodiments, the FOM is greater than or equal to 1.75. In some embodiments, the FOM is greater than or equal to 2.0. In some embodiments, the FOM is greater than or equal to 10.0. In some embodiments, the FOM merit ranges from 2.0 to 5.0.
  • the particle size distribution may be expressed by the following ratio: D90/D50, where D90 represents a particle size in which 90% of the volume of ATO nanoparticles have a diameter smaller than the stated D90; and D50 represents a particle size in which 50% of the volume of ATO nanoparticles have a diameter smaller than the stated D50.
  • D90/D50 is 1.5.
  • a composition with a lower D90/D50 will, in general, have a higher Figure-of-Merit.
  • the antimony tin oxide nanoparticles have a particle size distribution, as measured by the ratio of D90/D50, less than or equal to 2.0. In some embodiments, the particle size distribution is less than or equal to 1.5. In some embodiments, the particle size distribution ranges from 1.5 to 3.0. In some embodiments, the particle size distribution ranges from 1.75 to 2.25.
  • the ATO nanoparticles may have different average particle size.
  • the mean particle size equals less than 50 nm. In some embodiments, the mean particle size equals less than 20 nm. In some embodiments, the mean particle size ranges from 5 to 250 nm. In some embodiments, the mean particle size ranges from 30 to 100 nm. In some embodiments, the mean particle size ranges from 5 to 100 nm. In some embodiments, the mean particle size ranges from 5 to 30 nm. In some embodiments, the mean particle size ranges from 100 to 250 nm.
  • the ATO nanoparticles may be stoichiometric or non-stoichiometric.
  • the invention is a nanocomposite comprising any embodiment of the ATO nanoparticles in a medium suitable for energy transfer.
  • the medium suitable for energy transfer is an aqueous or solvent based ink or coating formulation.
  • the ink or coating is transparent, in other embodiments it is light colored.
  • the medium suitable for energy transfer is a polymer or a monomer.
  • the polymer in some embodiments, is any polymer that is suitable to produce a molded article or preform.
  • the monomers are likewise those monomers capable of making any polymer that is suitable to produce a molded article or a preform.
  • the polymers are selected from polyesters such as polycarbonate, polyethylene terephthalate (PET), and polyethylene naphthalate (PEN).
  • the medium suitable for energy transfer comprises a monomer used to make polyesters, such as polycarbonate, PET and PEN.
  • the polymers are copolyesters and blends of PET and PEN.
  • the medium suitable for energy transfer is a monomer or polymer that is a polyester, and in some embodiments (PET), (PEN) or copolyesters or blends of PET and PEN.
  • PET PET
  • PEN copolyesters or blends of PET and PEN.
  • the polyethylene terephthalate resin contains repeat units from at least 85 mole percent terephthalic acid and at least 85 mole percent ethylene glycol
  • the PEN resin contains repeat units from at least 85 mole percent 2,6-naphthalene- dicarboxlic acid and at least 85% ethylene glycol, based on 100 mole percent dicarboxylic acid and 100 mole percent diol.
  • the dicarboxylic acid component of the polyester may optionally be modified with up to about 15 mole percent of one or more different dicarboxylic acids other than terephthalic acid or suitable synthetic equivalents such as dimethyl terephthalate.
  • additional dicarboxylic acids include aromatic dicarboxylic acids preferably having 8 to 14 carbon atoms, aliphatic dicarboxylic acids preferably having 4 to 12 carbon atoms, or cycloaliphatic dicarboxylic acids preferably having 8 to 12 carbon atoms.
  • examples of dicarboxylic acids to be included with terephthalic acid are: phthalic acid, isophthalic acid, naphthalenedicarboxylic acid (including, but not limited to the 2,6-isomer), cyclohexanedicarboxylic acid, cyclohexanediacetic acid, diphenyl-4,4'- dicarboxylic acid, succinic acid, glutaric acid, adipic acid, azelaic acid, sebacic acid, and the like.
  • examples of dicarboxlic acids to be included with naphthalene-2,6-dicarboxylic acid are phthalic acid, terephthalic acid, isophthalic acid, other isomers of naphthlenedicarboxylic acid, cyclohexane-dicarboxylic acid, cyclohexanediacetic acid, diphenyl-4,4"-dicarboxylic acid, succinic acid, glutaric acid, adipic acid, azelaic acid, sebacic acid, and the like.
  • polyesters may be prepared from two or more of the above dicarboxylic acids. [0044] In some embodiments, it should be understood that use of the corresponding acid anhydrides, esters, and acid chlorides of these acids is included in the term "dicarboxylic acid.”
  • the polyester component may optionally be modified with up to about 15 mole percent, of one or more different diols other than ethylene glycol.
  • additional diols include cycloaliphatic diols preferably having 6 to 20 carbon atoms or aliphatic diols preferably having 3 to 20 carbon atoms.
  • diols to be included with ethylene glycol are: diethylene glycol, triethylene glycol, 1 ,4-cyclohexanedimethanol, propane- 1, 3 -diol, butane- 1,2-diol, pentane-l,5-diol, hexane-l,6-diol, 3-methylpentanediol-(2,4), 2-methylpentanediol- (1,4), 2,2,4-trimethylpentane-diol-(l,3), 2-ethylhexanediol-(l,3), 2,2-diethylpropane- diol-(l,3), hexanediol-(l,3), 1 ,4-di-(hydroxyethoxy)-benzene, 2,2-bis-(4-hydroxy- cyclohexyl)-propane, 2,4-dihydroxy-l,l,3,3-tetra
  • polyesters may be prepared from two or more of the above diols.
  • the polyethylene terephthalate resin may also contain small amounts of trifunctional or tetrafunctional comonomers such as trimellitic anhydride, trimethylolpropane, pyromellitic dianhydride, pentaerythritol, and other polyester forming polyacids or polyols generally known.
  • the PET polyesters comprise at least about 90 mole % terephthalic acid or dimethyl terephthalate and about 90 mole % ethylene glycol residues
  • polyethylene terephthalate based polyesters may be prepared by conventional polycondensation procedures well-known in the art.
  • such processes include direct condensation of the dicarboxylic acid(s) with the diol(s) or by ester interchange using a dialkyl dicarboxylate.
  • a dialkyl terephthalate such as dimethyl terephthalate is ester interchanged with the diol(s) at elevated temperatures in the presence of a catalyst.
  • the polyesters may also be subjected to solid state polymerization methods.
  • PEN polyesters may also be prepared by well known polycondensation procedures.
  • the medium suitable for energy transfer is chosen from organic polymers and organic monomers.
  • the organic polymers are chosen from polyesters.
  • the polyesters are chosen from polyethylene terephthalates.
  • the polymers are chosen from polypropylene and monomers thereof.
  • the polypropylene is biaxially oriented polypropylene.
  • the polymers and monomers are chosen from propylene homopolymers; random copolymers of propylene and ⁇ -olefms, which in some embodiments are ethylene; and propylene homopolymer/propylene- ⁇ -olefm copolymer.
  • the organic polymers and monomers are chosen from poly(ethylene terephthalate), polycarbonate, polypropylene, polyethylene, cyclic polyolefm's, Norborne polymers, polystyrene, syndiotactic polystyrene, styrene-acrylate copolymers, acrylonitrile- styrene copolymers, poly(ethylene naphthalate), polyethersulfone, polysulfone, polyamides, including nylons, poly(urethanes), acrylics, cellulose acetates, cellulose triacetates, vinyl chloride polymers, polyvinyl fluoride, polyvinylidene fluoride, poly(ethylene-co-vinyl acetate); ethyl acrylic acetate (EM); ethyl methacrylate (EMAC); metallocene-catalyzed polyethylene; plasticized poly(vinyl chloride); ISD resins; polyurethane; a
  • the polymers and monomers are chosen from resins, which, in some embodiments, may be chosen from any naturally occurring or synthetic polymer prepared by polymerization, polycondensation or polyaddition, such as polyethylene, polypropylene, polyisobutylene, polystyrene, polyvinyl chloride, polyvinylidene chloride, polyvinyl acetals, polyacrylonitrile, polyacrylates, polymethacrylates, polybutadiene, ABS, ethylene vinyl acetate, polyamides, polyimides, polyoxymethylene, polysulfones, polyphenylene sulfide, polycarbonates, polyurethanes, polyethers, polyether sulfones, polyacetals, phenolics, polycarbonate, polyester carbonate, polyethylene terephthalate, polybutylene terephthalate, polyarylates, polyether ketones, and blends thereof, copolymers thereof, and monomers thereof.
  • resins which, in some embodiments, may
  • the polymers and monomers are chosen from polyvinylbutyrals and monomers thereof.
  • the polyvinylbutyrals are chosen from those containing from about 17 to 23% by weight of vinyl alcohol units, and in some embodiments those containing from 20 to 21% by weight of vinyl alcohol units.
  • the medium suitable for energy transfer can also be formulated into coating compositions as is well known in the art and applied by known coating techniques to any type of substrate.
  • the substrate is chosen from plastic, metal, glass, ceramic, wood, upholstery, carpets, and textiles.
  • the substrate is coated, associated with adhesive, varnishes, papers, and/or inks.
  • one or more other ingredients may be added.
  • the one or more other ingredients are chosen from crystallization aids, impact modifiers, surface lubricants, denesting agents, stabilizers, antioxidants, ultraviolet light absorbing agents, deactivators, colorants, nucleating agents, fillers, acetaldehyde reducing compounds, other reheat enhancing aids, and anti-abrasion additives.
  • the polymer resin may also contain one or more branching agents, such as trifunctional and tetrafunctional comonomers such as trimellitic anhydride, trimethylol propane, pyromellitic dianhydride, pentaerythritol, and other polyester forming polyacids or polyols generally known in the art.
  • a variety of other articles can be made from any of the embodiments of the ATO nanoparticles and/or the nanocomposite comprising the ATO nanoparticles.
  • the articles are those in which reheat is neither necessary nor desirable.
  • articles include sheet, film, bottles, trays, other packaging, rods, tubes, lids, fibers and injection molded articles.
  • a beverage bottle containing and/or suitable for holding substances like a liquid.
  • a heat-set beverage bottle containing and/or suitable for holding beverages which are hot-filled into the bottle.
  • the bottle is containing and/or suitable for holding carbonated soft drinks.
  • the bottle is containing and/or suitable for holding alcoholic beverages.
  • a container containing a preform there is provided.
  • the medium suitable for energy transfer contains a plasticizers.
  • the plasticizer is dihexyl adipate, phosphoric acid ester and phthalic acid ester.
  • the plasticizer concentrations ranges up to 35% by weight of the mediums suitable for energy transfer.
  • the ATO nanoparticles may be made by any method.
  • One of skill in the art is readily aware of methods of forming nanoparticles. For example the following references, which are specifically incorporated herein by reference, all teach methods of forming nanoparticles that may be used to form IR absorbing nanoparticles: U.S. Patent No. 5,788,738 to Pirzada et al; U.S. Patent No.
  • the ATO nanoparticles may be made by a high temperature gas phase method.
  • Example high temperature processes include, but are not limited to, combustion processes, plasma processes, laser ablation processes, calcining and grinding processes and combinations of these processes.
  • the ATO nanoparticles may be made by a wet chemistry method.
  • Example wet chemistry processes include, but are not limited to, sol-gel processes, precipitation processes, wet grinding processes, inverse-micelle methods, and combinations of these processes. See, e.g., Beck and Siegel, "The Dissociative Adsorption of Hydrogen Sulfide over Nanophase Titanium Dioxide," J. Mater. Res., 7, 2840 (1992), and Steigerwald and Brus, "Synthesis, Stabilization, and Electronic Structure of Quantum Semiconductor Nanoclusters," Ann. Rev. Mater. ScL, 19, 471 (1989).
  • the ATO nanoparticles may be made by a method using organometallic containing liquids as precursors. See, e.g., U.S. Pat. No. 5,984,997 assigned on its face to Nanomaterials Research Corporation, now NanoProducts
  • the ATO nanoparticles may be made by a method utilizing chlorides. See, e.g., U.S. Pat. No. 6,695,907 assigned on its face to
  • the percentage of antimony in the ATO nanoparticles may be adjusted by routinely varying the amount of antimony to the reacting system.
  • the figure of merit may be adjusted by choosing the right combination of average particle size and the right antimony content.
  • the D90/D50 ratio may be determined by a photosedimentation technique, such as measured by the LumiSizer instrument, sold by Lumi GMBH. Also, in any of the embodiments, the D90/D50 ratio may be varied by operating the nanoparticle production process to ensure homogenous conditions within the particle forming region of the process..
  • the average size of the ATO nanoparticles may be determined by calculating the equivalent spherical diameter from the BET nitrogen surface area[ Adjustment technique depends strongly on the production process).
  • any embodiment of the ATO nanoparticles may be introduced to a medium suitable for energy transfer (The energy transfer is from the photoexcited ATO nanoparticles to the medium suitable for energy transfer.).
  • the introducing could be done by chemical or mechanical methods.
  • any embodiment of the ATO nanoparticles may be introduced to a polymer or introduced to monomers before or during their polymerization at a suitable time and location.
  • any embodiment of the ATO nanoparticles may be introduced to a polymer or introduced to a monomer by mechanical mixing, shaking, stirring, grinding, ultrasound, etc., with or without the aid of a solvent system.
  • the amount of ATO nanoparticles used in the medium suitable for energy transfer will depend upon the particular application, the desired reduction in reheat time, and the toleration level in optical properties. In some embodiments, the amount of ATO nanoparticles may be at least 0.5 ppm or at least 1 ppm or at least 5 ppm.
  • the amount may be at least 10 ppm, in some cases at least 20 ppm, or even at least 25 ppm. In some embodiments, the amount may be up to 500 ppm or more, or up to about 300 ppm, or up to about 250 ppm. In some embodiments, the amount may be up to 1,000 ppm, or up to 5,000 ppm, or even up to 10,000 ppm or the amount may even exceed 10,000 ppm.
  • the method by which the ATO nanoparticles are introduced to the medium suitable for energy transfer may be illustrated by the following.
  • the ATO nanoparticles may be added to a polymer reactant system, during or after polymerization, to a polymer melt, or to a molding powder or pellets or molten polyester in the injection-molding machine from which the bottle preforms are made.
  • the ATO nanoparticles may be added at locations including proximate the inlet to an esterification reactor, proximate the outlet of an esterification reactor, at a point between the inlet and the outlet of an esterification reactor, anywhere along a recirculation loop, proximate the inlet to a prepolymer reactor, proximate the outlet to a prepolymer reactor, at a point between the inlet and the outlet of a prepolymer reactor, proximate the inlet to a polycondensation reactor, or at a point between the inlet and the outlet of a polycondensation reactor, or at a point between the outlet of a polycondensation reactor and a die for forming pellets, sheets, fibers, or bottle preforms.
  • the ATO nanoparticles may be added to a polyester polymer, such as PET, and fed to an injection molding machine by any method, including feeding the ATO nanoparticles to the molten polymer in the injection molding machine, or by combining the ATO nanoparticles with a feed of PET to the injection molding machine, either by melt blending or by dry blending pellets.
  • the ATO nanoparticles may be supplied as-is, or in a concentrate form in a polymer such as PET, or as a dispersion in a liquid or solid carrier.
  • suitable carriers include polyethylene glycol, mineral oil, hydrogenated castor oil, and glycerol monostearate.
  • the ATO nanoparticles may be added to an esterification reactor, such as with and through the ethylene glycol feed optionally combined with phosphoric acid, to a prepolymer reactor, to a polycondensation reactor, or to solid pellets in a reactor for solid stating, or at any point in-between any of these stages.
  • the ATO nanoparticles may be combined with PET or its precursors as-is, as a concentrate containing PET, or diluted with a carrier.
  • the carrier may be reactive to PET or may be non-reactive.
  • the ATO nanoparticles, whether neat or in a concentrate or in a carrier, and the bulk polyester, may be dried prior to mixing together.
  • the ATO nanoparticles may be dried in an atmosphere of dried air or other inert gas, such as nitrogen, and if desired, under sub-atmospheric pressure.
  • the polyester compositions of the present invention may be used to form preforms used for preparing packaging containers.
  • the preform is typically heated above the glass transition temperature of the polymer composition by passing the preform through a bank of quartz infrared heating lamps, positioning the preform in a bottle mold, and then blowing pressurized air through the open end of the mold.
  • bottle preforms which are test-tube shaped injection moldings, are heated above the glass transition temperature of the polymer, and then positioned in a bottle mold to receive pressurized air through their open end.
  • This technology is well known in the art, as shown, for example in U.S. Pat. No. 3,733,309, incorporated herein by reference.
  • radiation energy from quartz infrared heaters is generally used to reheat the preforms.
  • the ATO nanoparticles can be made substantially transparent to visible light, addition of these particles to coatings, adhesives, varnishes, papers, and inks does not alter the transparency or color of these materials.
  • the small size of the ATO nanoparticles allows them to be distributed homogeneously in the coatings, adhesives, varnishes, papers, and inks and allows lower loading, which reduces costs.
  • the present invention provides coatings, adhesives, varnishes, papers, and inks comprising the ATO nanoparticles described herein.
  • the coatings, adhesives, varnishes, papers, and inks can contain one or more blends of ATO nanoparticles and/or composites comprising the ATO nanoparticles.
  • the ATO nanoparticles and/or composites comprising the ATO nanoparticles can be mixed with the coatings, adhesives, varnishes, papers, and inks or applied to the surface of the coatings, adhesives, varnishes, papers, and inks.
  • the ATO nanoparticles and/or composites comprising the ATO nanoparticles can be mixed with the coatings, adhesives, varnishes, papers, and inks during manufacturing or can be sprayed on the coatings, adhesives, varnishes, papers, and inks after they are applied to a substrate.
  • the ATO nanoparticles and/or composites comprising the ATO nanoparticles can be added at any time.
  • the ATO nanoparticles and/or composites comprising the ATO nanoparticles can be added by an end user, such as by mixing with the coating, adhesive, or ink or spraying the ATO nanoparticles and/or composites comprising the ATO nanoparticles on the coating, adhesive, or ink.
  • an end user such as by mixing with the coating, adhesive, or ink or spraying the ATO nanoparticles and/or composites comprising the ATO nanoparticles on the coating, adhesive, or ink.
  • One of skill in the art can readily select the amount of ATO nanoparticles and/or composites comprising the ATO nanoparticles to add to the composition depending on the particular application. For example, an curing or drying process required large amounts of IR energy may require addition of a large amount of ATO nanoparticles and/or composites comprising the ATO nanoparticles.
  • the IR absorption increases linearly as the amount of ATO nanoparticles is increased.
  • the ATO nanoparticles can be present in the coatings, adhesives, varnishes, papers, and inks in amount of less than 0.005 wt. %, less than 0.01 wt. %, less than 0.02 wt. %, or less than 0.1 wt. %.
  • the ATO nanoparticles can be functionalized depending on the particular application.
  • the ATO nanoparticles can be functionalized to bind or, in some embodiments, associate with a particular component of the coating, adhesive, or ink.
  • Such functionalization can speed polymerization by causing the ATO nanoparticles to associate with monomers to be polymerized.
  • the surface of the nanoparticles can be functionalized to be hydrophobic, hydrophilic, lipophilic, or lipophobic.
  • Such ATO nanoparticles can in some embodiments associate with some liquid component that is intended to be evaporated during drying.
  • the ATO nanoparticles can also be functionalized to facilitate their dispersion.
  • the ATO nanoparticles can be tailored to the particular application resulting in cheaper and more efficient use of coatings, adhesives, varnishes, papers, and inks.
  • the ATO nanoparticles may also absorb energy from parts of the electromagnetic spectrum other than infrared.
  • the ATO nanoparticles may also absorb ultraviolet energy. Nanoparticles that absorb both IR energy and UV energy may be used in application where the coating, adhesive, or ink should be resistant to UV energy. Because the ATO nanoparticles can also absorb UV in addition to IR energy, they may slow or prevent degradation commonly caused by UV radiation. The resulting coating or adhesive can also prevent heat from passing through the material.
  • IR absorbing nanoparticles that absorb both UV and IR energy can assist in curing or drying and improve the long-term performance of the coating, adhesive or ink.
  • the ATO nanoparticles absorb at least 50%, at least 75%, at least 85%, at least 90%, at least 95%, or at least 100% as much energy from a second portion of the UV electromagnetic spectrum as they absorb from the IR spectrum.
  • the ATO nanoparticles and/or composites comprising the ATO nanoparticles can be added to any type of coating, adhesive, or ink that can be cured or dried using IR energy.
  • the coating, adhesive, or ink must retain its optical properties, such as color and transparency.
  • the coating can be a clear coat or a color coat used in an automotive finishing process.
  • the ATO nanoparticles and/or composites comprising the ATO nanoparticles do not absorb significant amounts of light in the visible spectrum, they can be used in clear coat and color coat applications.
  • the ability of the ATO nanoparticles and/or composites comprising the ATO nanoparticles to transmit visible light also make them suited to use with inks.
  • Many adhesives must also retain one or more of their optical properties, such as retaining transparency, so ATO nanoparticles and/or composites comprising the ATO nanoparticles are also useful in these applications.
  • the present invention also provides methods of drying or curing coatings, inks, and adhesives using IR energy. Because the ATO nanoparticles absorb IR energy, the IR energy may be transferred to the medium suitable for energy transfer in the form of heat. Thus, the ATO nanoparticles and/or composites comprising the ATO nanoparticles can result in faster curing compared to curing coatings, inks, or adhesives without using the ATO nanoparticles and/or composites comprising the ATO nanoparticles. The method can also result in more efficient or effective curing compared to curing coatings, inks, or adhesives without using the ATO nanoparticles and/or composites comprising the ATO nanoparticles. Thus, the present invention provides an method of drying or curing coatings, inks, and adhesives that can speed processes, reduce costs, and result in coatings, inks, and adhesives with improves properties.
  • the method comprises contacting a coating, ink, or adhesive with the ATO nanoparticles and/or composites comprising the ATO nanoparticles and exposing the coating, ink, or adhesive to IR energy.
  • the contacting can occur in any manner.
  • the ATO nanoparticles can be mixed with at least one component of the coating, ink, or adhesive, such as one of more pigments, fillers, binders, solvents, or carriers.
  • many coatings, inks, and adhesives contain a polymer or similar material which functions as a binder for pigment or as the actual coating, ink, or adhesive itself.
  • the ATO nanoparticles and/or composites comprising the ATO nanoparticles can be dispersed into the monomer composition used to make the polymer, thereby achieving uniform dispersion throughout the polymer and intimate contact in the final formulation of the coating, ink, or adhesive.
  • the contacting can occur by applying the ATO nanoparticles and/or composites comprising the ATO nanoparticles to at least one surface of the coating, ink, or adhesive.
  • the ATO nanoparticles can be sprayed onto the coating, ink, or adhesive.
  • the contacting can also occur by applying the ATO nanoparticles and/or composites comprising the ATO nanoparticles to a substrate followed by applying the coating, ink, or adhesive to the substrate.
  • the ATO nanoparticles and/or composites comprising the ATO nanoparticles can be in powder form or dispersed into a solvent or carrier.
  • the contacting can occur by forming a film or sheet from the ATO nanoparticles and/or composites comprising the ATO nanoparticles.
  • This film or sheet can then be applied to the coating, adhesive, ink, or substrate followed by application of IR energy.
  • this film or sheet can be used multiple times.
  • the sheet or film can be prepared to match the shape of the substrate and used multiple times to apply one or more coatings, adhesives, varnishes, papers, and inks to the substrate.
  • the method comprises removing the ATO nanoparticles and/or composites comprising the ATO nanoparticles after some period of exposure to IR energy.
  • the ATO nanoparticles and/or composites comprising the ATO nanoparticles are formed into a film or sheet, this film or sheet can be removed once the IR energy has been applied.
  • the ATO nanoparticles and/or composites comprising the ATO nanoparticles can be simply washed off the surface of the coating, adhesive, or ink.
  • the ATO nanoparticles and/or composites comprising the ATO nanoparticles are not removed and remain a part of the coating, adhesive, or ink.
  • the IR energy can be applied in any manner.
  • the IR energy is applied using an IR heat source, such as an IR lamp.
  • IR lamps are commonly used and available to one of skill in the art.
  • Ambient IR energy is suitable.
  • the IR energy can also be applied by simply exposing the coating, adhesive, or ink to some other light source.
  • the other light source an be the light emitted by standard fluorescent lights or even sun light.
  • the IR energy can be supplied in any manner, as long as the IR energy is sufficient to at least partially affect the curing or drying.
  • the method can further comprise applying a second coating, adhesive, or ink.
  • This second coating can be the same or different than the first coating, adhesive, or ink.
  • the method comprises contacting the second coating, ink, or adhesive with the ATO nanoparticles and/or composites comprising the ATO nanoparticles and exposing the coating, ink, or adhesive to IR energy.
  • the method can comprise applying multiple coatings, adhesives, varnishes, papers, and inks, contacting one or more of the coatings, adhesives, varnishes, papers, and inks with ATO nanoparticles and/or composites comprising the ATO nanoparticles, and exposing the one or more of the coatings, adhesives, varnishes, papers, and inks to IR energy.
  • the ATO nanoparticles and/or composites comprising the ATO nanoparticles are used to facilitate laser marking of articles suitable for laser marking. See, e.g., U.S. Patent No. 7,187,396, assigned on its face to Engelhard Corporation, which patent is explicitly incorporated herein by reference.
  • the articles suitable for laser marking are chosen from plastic articles suitable for laser marking, which in some embodiments include any plastic articles that are molded, extruded or formed by any known conventional method.
  • the articles suitable for laser marking comprise the ATO nanoparticles and/or composites comprising the ATO nanoparticles and may or may not further comprise other additives.
  • the other additives are chosen from reinforcing fillers, flame retardants, antioxidants, dispersants, impact modifiers, ultraviolet stabilizers, plasticizers, and the like.
  • the ATO nanoparticles and/or composites comprising the ATO nanoparticles may be incorporated into plastic coatings, including coatings, varnishes, and inks. Such coatings or inks can be applied onto the surface of any article such as those formed of plastic, metal, glass, ceramic, wood.
  • plastic coatings containing the ATO nanoparticles and/or composites comprising the ATO nanoparticles make it possible to use of lasers to mark various types of substrates.
  • any laser can be employed.
  • the laser has a wavelength ranging from 780 nm to 2000 nm, or the range from 380 nm to 780 nm, or the range 150 nm to 380 nm (each wavelength includes harmonics and summing).
  • suitable lasers are chosen from solid state pulsed or cw lasers, pulsed or cw metal vapor lasers, excimer lasers and continuous wave lasers with pulse modification, such as the commercially available Nd: YAG laser (wavelength 1064 nm), frequency-doubled Nd: YAG laser (wavelength 532 nm plus other harmonics and sums), excimer laser (wavelengths depending on excimer, e.g., 193 nm, 351 nm, etc.), CO 2 laser (9.4-10.6 ⁇ m), titanium sapphire (from about 650 to 1100 nm)
  • 0.05 wt% nanoparticles dispersed in ethylene glycol measured at an infrared wavelength of 1100 nm, using a Perkin-Elmer spectrophotometer, operated in transmittance mode.
  • IR absorption properties of the materials Specifically, nanoparticles of reduced indium tin oxide (rITO) and antimony tin oxide (New Material) were prepared.
  • rITO reduced indium tin oxide
  • New Material antimony tin oxide
  • Carbon black was also used.
  • the materials were dispersed in ethylene glycol in differing percentages reduced indium tin oxide (0.025% and 0.05%), antimony tin oxide (0.1%), and carbon black (0.005%, 0.01%, 0.02%). Results are in Figure 1.
  • the 16% Sb antimony-doped tin oxide nanoparticles were used.
  • Table 2 shows the visible absorbance (extinction) of 0.05 wt% nanoparticles dispersed in ethylene glycol at a visible wavelength of 550 nm, using a Perkin-Elmer spectrophotometer, operated in transmittance mode.
  • Tables 1 and 2 show that an improved antimony tin oxide would have both a high antimony content, and a low particle size. This specific combination of particle size and particle composition is needed to give a high ratio of infrared absorbance to visible absorbance.

Abstract

Cette invention a trait à une nanoparticule d'oxyde d'antimoine et d'étain (ATO) utilisée pour le transfert d'énergie infrarouge, à ses composites, ses procédés d'utilisation et ses procédés de fabrication.
PCT/US2007/083779 2006-11-07 2007-11-06 Absorbeur d'infrarouge WO2008127409A2 (fr)

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