US20120128314A1 - D1451 methods for formulating radiation curable supercoatings for optical fiber - Google Patents

D1451 methods for formulating radiation curable supercoatings for optical fiber Download PDF

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US20120128314A1
US20120128314A1 US13/388,726 US201013388726A US2012128314A1 US 20120128314 A1 US20120128314 A1 US 20120128314A1 US 201013388726 A US201013388726 A US 201013388726A US 2012128314 A1 US2012128314 A1 US 2012128314A1
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supercoatings
optical fiber
primary
primary coating
layer
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Xiaosong Wu
Steven Robert Schmid
Timothy Edward Bishop
John Monroe Zimmerman
Wendell Wayne Cattron
Edward Joseph Murphy
Pratik Shah
Margaret Brumm
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DSM IP Assets BV
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    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/10—Coating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00—Processes for applying liquids or other fluent materials
    • B05D1/40—Distributing applied liquids or other fluent materials by members moving relatively to surface
    • B05D1/42—Distributing applied liquids or other fluent materials by members moving relatively to surface by non-rotary members
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/10—Coating
    • C03C25/104—Coating to obtain optical fibres
    • C03C25/1065—Multiple coatings
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/10—Coating
    • C03C25/12—General methods of coating; Devices therefor
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/10—Coating
    • C03C25/24—Coatings containing organic materials
    • C03C25/26—Macromolecular compounds or prepolymers
    • C03C25/32—Macromolecular compounds or prepolymers obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/62—Surface treatment of fibres or filaments made from glass, minerals or slags by application of electric or wave energy; by particle radiation or ion implantation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/48—Polyethers
    • C08G18/4866—Polyethers having a low unsaturation value
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/67—Unsaturated compounds having active hydrogen
    • C08G18/671—Unsaturated compounds having only one group containing active hydrogen
    • C08G18/672—Esters of acrylic or alkyl acrylic acid having only one group containing active hydrogen
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
    • C09D175/04—Polyurethanes
    • C09D175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
    • C09D175/16—Polyurethanes having carbon-to-carbon unsaturated bonds having terminal carbon-to-carbon unsaturated bonds
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/04—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of organic materials, e.g. plastics
    • G02B1/045—Light guides
    • G02B1/046—Light guides characterised by the core material
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
    • G02B6/02—Optical fibres with cladding with or without a coating
    • G02B6/02395—Glass optical fibre with a protective coating, e.g. two layer polymer coating deposited directly on a silica cladding surface during fibre manufacture
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2913—Rod, strand, filament or fiber
    • Y10T428/2933—Coated or with bond, impregnation or core

Definitions

  • the present invention relates to radiation curable coatings for optical fiber.
  • An optical fiber is a glass fiber that carries light along its length.
  • Optical fibers are widely used in fiber-optic communications, which permits transmission over longer distances and at higher bandwidths (data rates) than other forms of communications. Fibers are used instead of metal wires because signals travel along them with less loss, and they are also immune to electromagnetic interference.
  • MMF multi-mode fibers
  • SMF single-mode fibers
  • Attenuation in fiber optics also known as transmission loss, is defined as the reduction in intensity of the light beam (or signal) with respect to distance traveled through a transmission medium.
  • Attenuation loss coefficients in optical fibers usually are reported using units of decibels per kilometer, abbreviated dB/km.
  • Attenuation is an important factor limiting the transmission of a digital signal across large distances. Thus, much research has gone into both limiting the attenuation and maximizing the amplification of the optical signal. Empirical research has shown that attenuation in optical fiber is caused primarily by both scattering and absorption.
  • Microbends are sharp but microscopic curvatures in an optical fiber involving local axial displacements of a few micrometers and spatial wavelengths of a few millimeters. Microbends can be induced by thermal stresses and/or mechanical lateral forces. When present, microbeads attenuate the signal transmission capability of the coated optical fiber. Thus for the success of a telecommunications network it is known each telecommunications system has a limit to the amount of tolerable increase in attenuation for optical fiber and that to avoid reaching that limit it is well to reduce microbending overall because reducing microbending, reduces the increase in attenuation.
  • optical fiber coating technology One of the critical driving forces for the development of optical fiber coating technology is increased user demands on videos.
  • 2G network application is sufficient.
  • future networks such as 3G, 4G, and IPTV, high definition television (HDTV), video conferencing and other high bandwidth applications will impose a higher requirement for the performance of optical fiber, therefore the requirement of performance of the optical fiber coating will become higher and higher.
  • the Supercoatings comprise at least two layers, wherein the first layer is a Primary Coating that is in contact with the outer surface of the optical fiber and the second layer is a Secondary Coating in contact with the outer surface of the Primary Coating,
  • the cured Primary Coating on the optical fiber has the following properties after initial cure and after one month aging at 85° C. and 85% relative humidity:
  • Tube Tg of from about ⁇ 25° C. to about ⁇ 55° C.
  • the cured Secondary Coating on the optical fiber has the following properties after initial cure and after one month aging at 85° C. and 85% relative humidity:
  • Tube Tg of from about 50° C. to about 80° C.
  • the first aspect of the instant claimed invention is a method of formulating radiation curable Supercoatings for application to an optical fiber used in a telecommunications network, wherein said Supercoatings comprise at least two layers, the first layer being a primary coating that is in contact with the outer layer surface of the optical fiber and the second layer being a secondary coating in contact with the outer surface of the primary coating, wherein the cured primary coating on the optical fiber has the following properties after initial cure and after at least one month aging at 85° C. and 85% relative humidity:
  • the second aspect of the instant claimed invention is the Method of the first aspect, in which the Three-Dimensional Laced Methodology includes using a Multi-Layer Film Drawdown method to evaluate composite fused Primary Coating Layer and Secondary Coating Layer of Radiation curable Supercoatings.
  • composition of the Secondary Coating layer, prior to curing is selected from the group
  • composition of the Primary Coating layer, prior to curing is selected from the group
  • composition of the Secondary Coating layer, prior to curing is selected from the group
  • FIG. 1 is a diagram of historical depiction of formulation diagram for how typical formulating for optical fiber coatings has been done—illustrating the prior art. This is a comparative example, not an example of the instant claimed invention.
  • FIG. 2 is the first embodiment illustrating the three-dimensional laced methodology for formulating radiation curable Supercoatings for Optical Fiber.
  • FIG. 3 is the second embodiment illustrating the three-dimensional laced methodology for formulating radiation curable Supercoatings for Optical Fiber.
  • FIG. 4 is the third embodiment illustrating the three-dimensional laced methodology for formulating radiation curable Supercoatings for Optical Fiber.
  • FIG. 5 is an illustration of the results of the Multi-Layer Film Drawdown method showing a colored photograph of a Supercoatings Primary Layer, drawn down with a 1.5 mil bar, then a candidate for Supercoatings Secondary layer, observed as a brown layer, is drawn down over the primary with a 3 mil bar, and the whole plate cured.
  • FIG. 6 is Spectra “all”, which shows 4 spectra with a comparable appearance to two sets of two sitting on top of each other.
  • FIG. 7 is Spectra “Brown” shows the colored secondary portion only, and the top of the dual drawdown portion. The two spectra match up quite well.
  • FIG. 8 is Spectra “for the Supercoatings Primary Layer from Example 1PC1” shows the glass side of the dual layer, and the glass side of a single 3 mil, Example 1PC1 Supercoatings Primary Layer drawdown. Again the spectra match up very well.
  • FIG. 9 is a DMA plot of a Flat Film Drawdown of Primary PMoct Supercoatings Candidate, this is a Comparative Example, not an Example of the Instant Claimed Test Method.
  • FIG. 10 is a DMA plot of a Flat Film Drawdown of Secondary PMoct, Supercoatings Candidate, this is a Comparative Example, not an Example of the Instant Claimed Test Method.
  • FIG. 11 is a DMA plot of a Tube of Secondary PMoct, Supercoatings Candidate over Primary PMoct Supercoatings as put on wire using the Draw Tower Simulator; this is a Comparative Example, not an Example of the Instant Claimed Test Method.
  • FIG. 12 is a Dynamic Mechanical Analysis (“DMA”) plot of composite film of PMoct Primary (Example 1PB3) covered by PMoct Secondary (Example 2SB3) applied Wet-on-Wet (abbreviated W-O-W).
  • DMA Dynamic Mechanical Analysis
  • FIG. 13 is a DMA plot of composite film of PMoct Primary (Example 1PB3) covered by PMoct Secondary (Example 2SB3) applied Wet on Dry (abbreviated W-O-D).
  • the first aspect of the instant claimed invention is a method of formulating radiation curable Supercoatings for application to an optical fiber used in a telecommunications network, wherein said Supercoatings comprise at least two layers, the first layer being a primary coating that is in contact with the outer layer surface of the optical fiber and the second layer being a secondary coating in contact with the outer surface of the primary coating, wherein the cured primary coating on the optical fiber has the following properties after initial cure and after at least one month aging at 85° C. and 85% relative humidity:
  • the cured secondary coating on the optical fiber has the following properties after initial cure and after at least one month aging at 85° C. and 85% relative humidity:
  • said method comprising the steps of:
  • step f) using the results from step e)i) and step e)ii) to finalize the selection of Supercoatings to achieve the Maximum Acceptable Increase in Attenuation of the coated optical fiber.
  • the first step in the process is determining the Maximum Acceptable Increase in Attenuation requirements for the telecommunications network where the optical fiber will be installed. Determining the attenuation requirements for the telecommunications network involves the design criteria for the Optical Fiber Network. Some considerations in the design include: an understanding of how much of the network is straight line installation of multi-mode optical fiber as compared to how much of the network is Fiber-to-the-Home (abbreviated FFTH) installation of single mode optical fiber. There are many other design criteria for an Optical Fiber network that are known to people of ordinary skill in the art of designing Optical Fiber Networks.
  • Telecommunications Industry Association TIA
  • ICT information and communications technology
  • USTAG United States Technical Advisory Groups
  • IEC International Electrotechnical Commission
  • IEC International Electrotechnical Commission
  • Telcordia is a U.S. based corporation that provides fiber optic media & components analysis & consulting services. They also write and keep a library of Generic Requirements for Optical Fiber.
  • Method A Expandable Drum calls for at least 400 m of fiber to be wound with minimal tension around an expandable drum with material of fixed roughness on the drum surface.
  • Method B Fixed-Diameter Drum calls for at least 400 m of fiber to be wound with 3N tension around a fixed-diameter drum with material of fixed roughness on the drum surface.
  • Method C Wire Mesh calls for application of wire mesh (under load) to the fiber under Test.
  • Method D Baseketweave calls for 2.5 km of fiber to be applied to a fixed diameter drum via a “basketweave” wrap.
  • Method D specifically describes a procedure to measure the microbending sensitivity of fibers as a function of temperature and provides the microbending sensitivity over a wide temperature range and suggests that temperature cycling could include lower temperatures such as ⁇ 60° C.
  • microbending sensitivity using test Method D Baseweave will be spoken of in terms of a dB/Km number, at a specified wavelength and temperature.
  • Method D measured Microbending Sensitivity will be discussed and reported in units of attenuation which will be spoken of in terms of a dB/Km number, at a specified wavelength and temperature. It is understood that whatever Microbending Sensitivity is given, that the number given is the Maximum Acceptable Increase in Attenuation permissible for that optical fiber in a given telecommunications network.
  • Method D specifically describes a procedure to measure the Microbending Sensitivity of fibers as a function of temperature and provides the Microbending Sensitivity over a wide temperature range and suggests that temperature cycling could include lower temperatures such as ⁇ 60° C.
  • Microbending Sensitivity as a change in attenuation from a baseline per the IEC procedure; this procedure requires the reporting of change in attenuation be reported at specific wavelengths and a temperature of ⁇ 60° C. Applicants believe that reporting Microbending Sensitivity data at these extreme temperature conditions will provide a type of “worst case scenario” possibility for Microbending Sensitivity of the coated optical fiber in the field.
  • Microbending Sensitivity testing it may or may not be possible to identify the difference in Microbending Sensitivity between an Optical Fiber coated with a standard, “non-Supercoatings” coating, because neither Supercoatings or a non-Supercoatings is anywhere near their glass transition temperature (Tg) for the primary coating layer at room temperature.
  • Tg glass transition temperature
  • the Telecommunications network generally requests that Optical Fiber be supplied with a known maximum attenuation at 1310 nm and room temperature. This highest tolerable level of attenuation is known to people of ordinary skill in the art of design criteria for Telecommunications networks.
  • Optical Fibers coated with Radiation curable Supercoatings it is possible and desirable to report Microbending Sensitivity at three separate wavelengths and at a very cold ( ⁇ 60° C.) temperature. This data can then be used by the Network designer to understand the limits, and be able to predict failure modes for the network. It is applicants' position that a network containing Optical Fibers coated with standard, “non-Supercoatings” will have much less tolerance to the stress involved from the cable environment of temperature extremes and mechanical forces than will a network containing Optical Fibers coated with Radiation curable Supercoatings.
  • the next step in the process is determining the Field Application Environment of the Supercoatings requirements for the telecommunications network where the optical fiber will be installed.
  • the Field Application Environment involves the understanding of four factors:
  • Optical Fiber is known to have standard grades for installation of long haul straight cable. Recently various grades of “bend resistant” Optical Fiber have been developed by Optical Fiber Suppliers such as Corning and Draka and OFS and YOFC and others. These bend resistant Optical Fibers are being deployed in Fiber to the Node (FTTX) and Fiber to the Home (FTTH) applications.
  • FTTX Node
  • FTTH Fiber to the Home
  • Current commercial Optical Fiber available for sale include: Corning® InfiniCor® optical fibers, Corning® ClearCurve® OM2/OM3/OM4 multimode optical fiber, Corning® ClearCurve® single-mode optical fiber, Corning® SMF-28e® XB optical fiber, Corning® SMF-28® ULL optical fiber,
  • BB Draka BendBright SingleMode
  • TM Draka TeraLight Singlemode
  • TU Draka TeraLight Ultra Singlemode
  • BX Draka BendBright-XS
  • LA Draka Enhanced Single Mode
  • NZDSF-LA Singlemode Draka NZDSF-LA Singlemode
  • OFS HCS®, OFS FiberWire®, and OFS PYROCOAT® brand technologies YOFC HiBand GIMM fiber, YOFC High Temperature Fibre (HTF) Series, YOFC HiBand Graded-Index Multimode Optical Fiber (50/125 & 62.5/125 um) and others.
  • the formulator of Supercoatings in order to produce an optical fiber with the desired attenuation properties it is desirable, optionally even necessary, for the formulator of Supercoatings to have an understanding of the details of the optical fiber production process. These details include the type of glass, the processing temperature, the atmosphere surrounding the application of coating(s), the line speed, the type of radiation source, typically described as a “curing lamp”, and the location and number of curing lamps along the processing line and whether the secondary coating is applied over the primary coating wet on wet or wet on dry. These types of mechanical aspects to the glass processing have, in the past, not been of interest to the formulator of the Optical Fiber coatings because the formulator focused on the Optical Fiber coatings and the glass manufacturer focused on the glass.
  • UV mercury arc lamps emit light by using an electric arc to excite mercury that resides inside an inert gas (e.g., Argon) environment to generate ultraviolet light which effectuates curing.
  • inert gas e.g., Argon
  • microwave energy can also be used to excite mercury lamps in an inert gas medium to generate the ultraviolet light.
  • arc excited and microwave excited mercury lamp, plus various additives (ferrous metal, Gallium, etc.) modified forms of these mercury lamps are identified as mercury lamps.
  • Conventional ultraviolet mercury arc lamps are the “state-of-the-art” when it comes to curing of radiation curable coatings for optical fiber.
  • ultraviolet mercury lamps as a radiation source suffers from several disadvantages including environmental concerns from mercury and the generation of ozone as a by-product. Further, mercury lamps typically have lower energy conversion ratio, require warm-up time, generate heat during operation, and consume a large amount of energy when compared with Lights that are generated by Light Emitting Diodes “LED”.
  • LEDs In contrast to ultraviolet mercury lamps, light emitting diodes (LEDs) are semiconductor devices which use the phenomenon of electroluminescence to generate light. LEDs consist of a semiconducting material doped with impurities to create a p-n junction capable of emitting light as positive holes join with negative electrons when voltage is applied. The wavelength of emitted light is determined by the materials used in the active region of the semiconductor. Typical materials used in semiconductors of LEDs include, for example, elements from Groups 13 (III) and 15 (V) of the periodic table. These semiconductors are referred to as III-V semiconductors and include, for example, GaAs, GaP, GaAsP, AlGaAs, InGaAsP, AlGaInP, and InGaN semiconductors. Other examples of semiconductors used in LEDs include compounds from Group 14 (IV-IV semiconductor) and Group 12-16 (II-VI). The choice of materials is based on multiple factors including desired wavelength of emission, performance parameters, and cost.
  • LEDs used gallium arsenide (GaAs) to emit infrared (IR) radiation and low intensity red light. Advances in materials science have led to the development of LEDs capable of emitting light with higher intensity and shorter wavelengths, including other colors of visible light and UV light. It is possible to create LEDs that emit light anywhere from a low of about 100 nm to a high of about 900 nm.
  • known LED UV light sources emit light at wavelengths between about 300 and about 475 nm, with 365 nm, 390 nm and 395 nm being common peak spectral outputs. See textbook, “Light-Emitting Diodes” by E. Fred Schubert, 2 nd Edition, ⁇ E. Fred Schubert 2006, published by Cambridge University Press.
  • LED lamps offer advantages over conventional mercury lamps in curing applications. For example, LED lamps do not use mercury to generate UV light and are typically less bulky than mercury UV arc lamps. In addition, LED lamps are instant on/off sources requiring no warm-up time, which contributes to LED lamps' low energy consumption. LED lamps also generate much less heat, with higher energy conversion efficiency, have longer lamp lifetimes, and are essentially monochromatic emitting a desired wavelength of light which is governed by the choice of semiconductor materials employed in the LED.
  • LED lamps for commercial curing applications. For example, Phoseon Technology, Summit UV Honle UV America, Inc., IST Metz GmbH, Jenton International Ltd., Lumios Solutions Ltd., Solid UV Inc., Seoul Optodevice Co., Ltd, Spectronics Corporation, Luminus Devices Inc., and Clearstone Technologies, are some of the manufacturers currently offering LED lamps for curing ink-jet printing compositions, PVC floor coating compositions, metal coating compositions, plastic coating composition, and adhesive compositions.
  • FIG. 1 is a diagram of historical depiction of formulation diagram for how typical formulating for optical fiber coatings has been done—illustrating the prior art.
  • Decision Chart 10 shows the two-dimensional Prior Art approach to formulating optical fiber coatings.
  • desirable functional property A is illustrated by circle A
  • Review Point B represents the test to determine whether the liquid optical fiber coating or the cured coating, either in the form of a flat film or in the form of a tubular coating on the optical fiber, has the desired functional property. If the optical fiber coating does have the desired functional property than the decision tree goes to yes and the inquiry is over. If the optical Fiber coating does not have the desired functional property, the formulator reviews the formulation and determines the change to make, as represented by parallelogram D, and then in rectangle C, the formulation is changed. The functional property is retested at Review Point B, and if the desired functional property is obtained then the inquiry is over.
  • the decision tree goes back to the top and other reformulating options by the formulator are considered until the next possible formulation is determined and then the formulation is changed and then the desired functional property is retested. This continues until the desired physical property is obtained.
  • Table 1A, 1B, 1C, 1D, 1E, 2A, 2B, 2C, 2D, 2E, 1F, 2F, 1G, 2G, 1H, 2H, 1J, and 2J which summarize the state-of-the-art understanding of the ingredients that may or may not be used in formulating Primary and Secondary Radiation Curable Coatings for optical fiber with respect to creating formulations with physical properties of the Primary Coating Layers and Secondary Coating Layers on the Optical Fiber that meet the rigorous criteria of Supercoatings.
  • additional information may be found in issued patents, published patent applications, scientific papers and other information commonly known to people of ordinary skill in the art of Radiation Curable Coatings for Optical Fiber.
  • vinyl ether many polyols and acids available, hydrolytic stability, (meth)acrylamide, vinyl amide oxidative stability more difficult to manufacture 3.
  • hydrocarbon e.g. other UV-curable end-groups very low Tg, hydrophobic, hydrolytic poorer oxidative polybutadiene
  • vinyl ether stability, low viscosity stability, poorer (meth)acrylate (meth)acrylamide, vinyl amide solubility, lipophilic 5.
  • thiol-ene various enes including, strong network structure, low odor, shelf stability norbornene, vinyl ether, vinyl viscosity, good cured stability ester, vinyl amide, allyl ether, allyl ester, allyl amide, styrene, alkenes (aliphatic enes are used for low Tg) Chemistry of Oligomer 7.
  • UV-curable end-groups or copolymer e.g. vinyl ether, (meth) acrylamide, vinyl amide 8.
  • cationic epoxy various cationically curable low shrinkage, good adhesion, low slower cure speed, post groups including glycidyl viscosity, stability curing effect, lower ether, glycidyl ester, vinyl elongation ether, oxetane, hydroxyl (aliphatic materials are used for low Tg)
  • silicone aliphatic, aromatic, linear, hydrophobic and lipophobic, expensive, refractive branched stability, low viscosity index may be too low 6.
  • fluorocarbon aliphatic, aromatic, linear, hydrophobic and lipophobic, expensive, refractive branched stability, low viscosity index may be too low 7.
  • DESMODUR ® W* bis(4- Polyurethane resins based on non-homogenous isomer isocyanotocyclohexyl) *Desmodur ® W diisocyanate have blending may lead to methane a high degree of flexibility coupled reproducibility issues for also known as PICM, with good mechanical strength.
  • HMDI hydrogenated MDI
  • a unique feature of lead to unexpected dicyclohexylmethane *Desmodur ® W diisocyanate is its performance properties of diisocyanate ability to form optically clear formulated coating polyurethanes when combined with suitable polyol coreactants.
  • TDI toluene diisocyanate
  • MDI is methylenebis(phenyl isocyanate)
  • Methyl Di-P-Phenylene Isocyanate IPDI is isophorone diisocyanate
  • HDI is Hexamethylene diisocyanate
  • TMDI is Trimethyl hexamethylene diisocyanate
  • TMXDI is TMXDI ® (Meta) Aliphatic Isocyanate, available from Cytec Industries Inc.
  • vinyl ether good chemical resistance generally high viscosity (meth)acrylamide, vinyl amide 7.
  • thiol-ene various enes including, strong network structure, low odor, shelf stability norbornene, vinyl ether, vinyl viscosity, good cured stability ester, vinyl amide, allyl ether, allyl ester, allyl amide, styrene, alkenes (aromatic or cyclic enes for higher Tg) 8.
  • cationic epoxy various cationically curable low shrinkage, good adhesion, slower cure speed, post groups including glycidyl low viscosity, stability curing effect, lower ether, glycidyl ester, vinyl elongation ether, oxetane, hydroxyl (aromatic materials for higher Tg)
  • alkyl (meth)acrylate generally low Tg, hydrophobic, good odor, slower cure speed, may be crystalline, stability, low cost, good diluent (generally volatile under high heat output of conventional monofunctional monomer used for lower mercury UV lights crosslink density and modulus)
  • aryl or cyclic (meth)acrylate generally higher Tg, hydrophobic may be volatile or crystalline 3.
  • ether (meth)acrylate generally low Tg, fast cure speed, generally more hydrophilic, poorer oxidative stability good diluent, aromatics have good dry adhesion (generally monofunctional monomer used for lower crosslink density and modulus) 4.
  • hydroxyl-functional, acid- good dry adhesion, fast cure speed generally higher Tg, more hydrophilic, can react functional, and other polar (generally monofunctional monomer used with other coating components monomers for lower crosslink density and modulus) 5.
  • (meth)acrylamides and vinyl good dry adhesion, fast cure speed generally higher Tg, more hydrophilic amides (generally monofunctional monomer used for lower crosslink density and modulus)
  • phenoxy ethyl (generally multifunctional monomer used acrylate, are volatile under high heat output for higher crosslink density and modulus) of conventional mercury UV lights or crystalline; therefore when an aryl reactive diluent monomer is present that has a molecular weight less than about 300, it should be present at no more than about 10 wt. % of the total formulation 3.
  • ether (meth)acrylate good stress-relaxation if branched, fast cure more hydrophilic, poorer oxidative stability speed, generally good diluent (generally multifunctional monomer used for higher crosslink density and modulus) 4.
  • FIG. 2 illustrates step 2 is the first aspect of the instant claimed invention method for formulating Supercoatings for Optical Fiber.
  • FIG. 2 shows six Decision Charts, 10 , 20 , 30 , 40 , 50 and 60 linked together in a three dimensional model by linking lace 307 .
  • Linking Lace 307 illustrates that any formulation change made in either the Primary Coating Layer or the Secondary Coating Layer of an Optical Fiber Supercoatings means that the other desired properties of an Optical Fiber Supercoatings must be tested after the initial change has been made, in order to be certain that one or more changes in the formulation don't lead to a negative influence on one or more functional properties of the Primary Coating Layer and Secondary Coating Layer.
  • the cured Primary Coating on the optical fiber has the following properties after initial cure and after one month aging at 85° C. and 85% relative humidity:
  • Tube Tg of from about ⁇ 25° C. to about ⁇ 55° C.
  • the cured Secondary Coating on the optical fiber has the following properties after initial cure and after one month aging at 85° C. and 85% relative humidity:
  • Tube Tg of from about 50° C. to about 80° C.
  • Step ii) of the instant claimed invention shows that any formulation change made to affect one of these six properties, means that all of the other five functional properties must be tested as well, to make sure that changing one aspect of the Supercoatings does not affect the other five aspects.
  • FIG. 3 shows the second embodiment of step ii) of the instant claimed method for formulating Supercoatings for Optical Fiber.
  • the possible changes involving reformulation of a Primary Coating Layer or Secondary Coating Layer of Supercoatings must be tested against each other to see if one change to achieve a desired functional property could also cause other changes that would negate a desired functional property.
  • FIG. 4 shows the third embodiment of step ii) of the instant claimed method for formulating Supercoatings for Optical Fiber.
  • the possible changes are linked by linking laces both horizontally and vertically amongst the six necessary functional Supercoatings properties. This linkage of properties is the essence of what makes Supercoatings for Optical Fibers different from simply a primary coating covered by a secondary coating layer.
  • the reality is that instead of formulating the Primary and Secondary coating layers separately from each other, that any formulation change in one of the layers, must be tested against all the properties required of the Supercoatings.
  • the second aspect of the instant claimed invention is the Method of the first aspect of the instant claimed invention, in which the Three-Dimensional Laced Methodology includes using a Multi-Layer Film Drawdown method to evaluate composite fused Primary Coating Layer and Secondary Coating Layer of Radiation curable Supercoatings.
  • FIG. 5 shows one such Film.
  • the Multi-Layer Film Drawdown method flat plate substrate method for evaluation of layers of potential Radiation curable Supercoatings-Primary and Secondary Layers comprises the following steps:
  • test coatings are most typically inner primary coatings.
  • a second drawdown is made over the top and wide enough to cover the edges of the first drawdown films.
  • This second drawdown is also made with a Bird type bar calibrated to deposit a film of typically 75 ⁇ to 254 ⁇ .
  • One such Bird type bar for the second layer has a film deposit height of 3.0 mils.
  • the glass plate with the two drawdowns and the consequent composite films is exposed to suitable actinic radiation to achieve the desired degree of cure. This method is known as the wet-on-wet method.
  • wet-on-dry method A similar method known as wet-on-dry method, is conducted in the same manner as the wet-on-wet method described above; except the first drawdown films are exposed to actinic radiation to effectuate the cure of the Primary Coating Layer. After this radiant exposure the second drawdown is made and the plate is then further exposed to radiation to effectuate the cure of the Secondary Layer and the Primary Layer into a Fused Composite film.
  • the method is used to apply some small dots of primary to a glass plate and drawdown with a 1 mil or 1.5 mil Bird Bar. While the primary is still uncured, a second drawdown of a colored secondary coating layer is made over the primary coating layer but with a 3 mil bar. The result is observed to be acceptably uniform as can be seen in FIG. 5 .
  • the Supercoatings Primary Layer is drawn down with a 1.5 mil bar, then a candidate for Supercoatings Secondary layer, observed as a brown layer, Example 3SA3 Color twoH, ⁇ Color 2HBrown ⁇ is drawn down over the Supercoatings Primary with a 3 mil bar. After this wet-on-wet application, the plate is exposed to radiation sufficient to effectuate the cure of both the Primary Coating Layer and the Secondary Coating Layer into a Fused Composite Film.
  • the Fused Composite film appears to be very uniform with the darker areas being 3 mil of colored secondary, and the lighter areas 1.5 mil each of primary and colored secondary over the top.
  • the Fused Composite film is easily removable and hand able for measurements of thickness and % RAUs, a critical measurement for both layers of Supercoatings for Optical Fiber.
  • FIGS. 7 , 8 and 9 The lack of mixing of the layers is further illustrated in FIGS. 7 , 8 and 9 .
  • FIG. 7 is Spectra “all”, which shows 4 spectra with a comparable appearance to two sets of two sitting on top of each other.
  • FIG. 8 is Spectra “Brown” showing the colored secondary portion only, and the top of the dual drawdown portion. The two spectra match up quite well.
  • FIG. 9 is Spectra “formulation Option A for the Supercoatings Primary Layer from Example 3SA3 Color twoH, ⁇ Color 2HBrown ⁇ ” showing the glass side of the dual layer, and the glass side of a single 3 mil Example 3 Supercoatings Primary Layer drawdown. Again the spectra match up very well.
  • This method permits the investigation of the properties of primary and secondary as a composite Supercoatings film in ways not available in the past. With this method it is now possible to conduct feasibility studies of Supercoatings Candidate Secondary Layers over Supercoatings Candidate Primary Layers for tensile properties, DMA characteristics, environmental durability, etc., with easily handled films instead of having to use the Draw Tower Simulator.
  • the Multi-layer Film Drawdown method including, but not limited to the following: the film drawdown takes away the line speed as a factor in coatings functionality to allow for more basic analysis; it also allows the formulator to evaluate the migration of materials from layer to layer during the wet on dry and wet on wet processing steps.
  • Multi-Layer Film Drawdown method Another advantage of the Multi-Layer Film Drawdown method is that it is critical for both wet on wet processing and wet on dry processing that sufficient through cure is possible to cure the primary coating to the requisite percentage RAU when the coating is applied to wire or optical fiber.
  • the primary coating may be undercured to achieve line speed with the expectations that the cure will be finished in the primary coating when the radiation is applied to the secondary coating. Therefore use of the Multi-Layer Film Drawdown method is helpful to simulate wet on wet application as compared to wet on dry application and testing the % RAU to determination of cure of primary through the secondary. The simulation allows the formulator to quickly evaluate the efficacy of different photoinitiators.
  • Multi-layer film drawdown method Another benefit of the Multi-layer film drawdown method is approximating the composite behavior of the cured secondary coating layer over the cured primary coating that can be correlated with Primary and Secondary characteristics that can be defined in SUPERCOATINGS. It is possible to evaluate the functional properties of each coating layer by analyzing film using solid film rheology testing, otherwise known as DMA (dynamic Mechanical Analysis)
  • CN-120Z epoxy diacrylate available from Sartomer.
  • DBTDL dibutyl tin dilaurate available from OMG Americas.
  • HEA hydroxyethyl acrylate available from BASF HHPA hexahydrophthalic anhydride, available from Milliken Chemical.
  • SR-506 isobornyl Acrylate, available as from Sartomer.
  • the present invention is further illustrated with a number of examples.
  • dB/Km less than about 0.15 at 1625 nm and ⁇ 60° C.
  • the radiation curable Radiation curable Supercoatings is applied Wet on Dry.
  • the curing lights available are: 600 w/10 inch D Lamps.
  • the line speed at which the Supercoatings will be applied is about 1400 m/minute.
  • Each Primary Coating Formulator selects the raw materials for their starting Oligomer, then the photoinitiator(s), antioxidant, one or more diluent monomers and other additives based on information available.
  • the oligomer synthesis is carried out as follows:
  • Oligomers suitable for coating compositions of the invention are prepared by reaction of at least one polyether polyol, at least one diisocyanate, at least one hydroxyl terminated acrylate or (meth)acrylate, and optionally an alcohol.
  • the following oligomer synthesis methods illustrate two different methods for synthesizing the oligomer. However, it will be appreciated by the skilled artisan that other synthesis methods also can be used so long as the oligomer comprises a urethane-backbone, with at least one terminal unsaturated group such as an alkenyl group or vinyl group.
  • Method A is also known as an “outside-in” method that first reacts the isocyanate with hydroxyl terminated acrylate or methacrylate, followed by the reaction with polyol.
  • Method B is also known as an “inside-out” method that first reacts the isocyanate with polyol, followed by the reaction with hydroxyl terminated acrylate or methacrylate.
  • Catalyst is added to a mixture of diisocyanate, polyol and inhibitor. The mixture is allowed to react at 60° C. for 2 h, so that the desired NCO content is reached. Then, HEA is added, and the mixture is allowed to react at 85° C. for 1 h or longer, until the NCO content is not greater than 0.05.
  • Polyether polyols suitable for preparing oligomers in accordance with the invention preferably are selected from the group consisting of a polyethylene glycol and a polypropylene glycol.
  • the polyether polyol is a polypropylene glycol.
  • Catalysts for synthesizing urethane based oligomers for use in radiation curable coatings for optical fiber are known in the art.
  • the catalyst is selected from the group consisting of copper naphthenate, cobalt naphthenate, zinc naphthenate, triethylamine, triethylenediamine, 2-methyltriethyleneamine, dibutyl tin dilaurate (DBTDL); metal carboxylates, including, but not limited to: organobismuth catalysts such as bismuth neodecanoate, CAS 34364-26-6; zinc neodecanoate, CAS 27253-29-8; zirconium neodecanoate, CAS 39049-04-2; and zinc 2-ethylhexanoate, CAS 136-53-8; sulfonic acids, including but not limited to dodecylbenzene sulfonic acid, CAS 27176-87-0; and methane s
  • Type I photoinitiators undergo a uni-molecular bond cleavage upon irradiation to yield free radicals
  • Type II photoinitiators undergo a bimolecular reaction where the excited state of the photoinitiator interacts with a second molecule (a co-initiator) to generate free radicals.
  • UV photoinitiators of both Type I and Type II are available.
  • Each Secondary Coating Formulator selects the raw materials for their starting Oligomer, then the photoinitiator(s), antioxidant, one or more diluent monomers and other additives based on information available.
  • each Secondary Coating Formulator takes into account the following: TDI Type II is inexpensive, and is a fast reacting isocyanate. Further to the selection of TDI Type II for use in Secondary Coatings, group contribution theory (takes the characteristics of each part of the group and contributes) teaches that the aromatic group in the isocyanate contributes to high Tg and high modulus in the secondary, which is a technical reason why aromatic isocyanates would be favored for secondary coatings.
  • BHT Food Grade Antioxidant scavenges free radicals ⁇ which is important because HEA (inhibited by methyl hydroquinone) can self-polymerize ⁇ ; therefore a synthetic chemist plans the synthesis to have the BHT in the reaction mixture before the HEA
  • the scavenging reaction also requires the presence of oxygen—it is known that the oxygen in normal ambient air is typically sufficient for this purpose.
  • 2-HEA (2-hydroxy ethyl acrylate) is a simple acrylate which historically has yielded very good cure rates in formulated radiation curable coatings for optical fiber.
  • HBA hydroxy butyl acrylate
  • HPA hydroxylethyl acrylate
  • Both the Primary Coating Formulators and the Secondary Coating Formulators are aware of the following as they formulate; the polymerization of the secondary coating layer causes shrinkage of that layer and the shrinkage of the secondary coating layer puts pressure on the primary coating layer, whether the primary coating layer is already cured or is in the process of being cured when the secondary coating layer is being cured. Stress relaxation is a measure of the relief of stress on the primary caused by the shrinkage of the secondary coating as the secondary coating polymerizes.
  • the temperature of the polymerization of the Secondary Coating Layer of a Supercoating has to be above the Tg for fast relief of that shrinkage.
  • the fiber cabler desires that the optical fiber is in a relaxed state before the optical fiber is manipulated further during the cabling process.
  • the formulators select materials that are more flexible in the secondary coating; however, these flexible materials must be selected in such a way that the additional flexibility does not negatively interfere with targeted physical properties of high Tg and high strength.
  • composition of the Primary Coating layer, prior to curing is selected from the group
  • composition of the Secondary Coating layer, prior to curing is selected from the group
  • the Single Mode Optical Fiber is of the most modern type, able to resist Microbending.
  • dB/Km less than about 0.05 at 1625 nm and ⁇ 60° C.
  • the Single Mode Optical Fiber is of the most modern type, able to resist Microbending
  • the radiation curable Radiation curable Supercoatings is applied Wet on Dry.
  • the number of curing lights are: from 1 to 3 in the Primary Coatings area,
  • the type of curing lights for the secondary coating are: 600 w/10 inch D Lamps
  • the line speed at which the Supercoatings will be applied is approximately 1300 m/min.
  • the fourth aspect of the instant claimed invention is a single-mode optical fiber coated with Supercoatings, wherein said Supercoatings comprise,
  • composition of the Primary Coating layer, prior to curing is selected from the group consisting of the formulations of Examples 1PA2, 1PB3, 1PC1, 2Alpha, 2Beta; and wherein the composition of the Secondary Coating layer, prior to curing, is selected from the group consisting of the formulations of Examples 2SA4 and 2SB3 and 5SA1.
  • dB/Km less than about 0.09 at 1625 nm and ⁇ 60° C.
  • the Single Mode Optical Fiber is of the most modern type, able to resist Microbending
  • the radiation curable Radiation curable Supercoatings is applied Wet on Wet.
  • the number of curing lights is: 3 lamps/20 inch.
  • a Multilayer Film DrawDown is made of a Primary Coating Layer and a Colored Secondary made of the Clear Secondary Coating and Colorant.
  • Oligomer M3 ⁇ is an Oligomer.
  • the ingredients combined to make Oligomer M3 include the following:
  • Oligomer M3 Material description Wt. % TDI Type ll 21.26 BHT Food Grade 0.05 2-HEA 14.18 Dibutyltin Dilaurate 0.05 Pluracol P1010 64.46 Total (due to rounding of significant 100.00 figures may be +/ ⁇ 0.10 wt.
  • the MULTI-Mode Optical Fiber is of the most modern type, able to resist Microbending
  • the radiation curable Secondary Coating is applied Wet on Wet Primary Coating.
  • the line speed at which the Primary Coating and Secondary Coating will be applied is about 200 meters/minute.
  • the Secondary Coating is a Clear Secondary.
  • the type of curing lights are: 600 w/ D Lamps.
  • an Oligomer is selected, along with a photoinitiator, antioxidant, two diluent monomers and other additives based on information available to make a Multi-Mode Coating.
  • an Oligomer Blend is selected, along with a photoinitiator, antioxidant, two diluent monomers and other additives based on information available to formulate a Clear Secondary Coating for Multi-Mode Coating.
  • the fifth aspect of the instant claimed invention is a multi-mode optical fiber coated with radiation
  • curable coatings comprising a Primary Coating Layer and a Secondary Coating Layer
  • composition of the Secondary Coating layer, prior to curing is selected from the group
  • This Supercoatings Secondary is formulated from an existing Supercoatings Secondary to meet the needs of a customer that is requesting a product with a higher refractive index to enable them to use installed equipment to ascertain concentricity in their finished coated fiber.
  • the changes from the earlier coating are as follows:
  • Example Example Example 5SA1 5SA2 5SA3 Function in Wt. % in Wt. % in Wt. % in Formula COMPONENT formula formula formula formula oligomer Oligomer M3 ⁇ 28.1 25.1 35.0 epoxy acrylate CN-110 37.4 39.4 37.4 acrylate monomer HDDA 5.2 5.2 5.2 acrylate monomer SR-601 10.3 10.3 10.3 acrylate monomer PEA 14.75 15.75 7.85 Photo initator TPO 0.75 0.75 0.75 Photo initiator Chivacure 184 2.5 2.5 2.5 2.5 Stabilizer Irgacure 1035 0.5 0.5 0.5 silicon surfactant DC-190 0.33 0.33 0.33 Silicon Surfactant DC-57 0.17 0.17 0.17 Total (due to 100 100 100 rounding of significant figures may be +/ ⁇ 0.10 wt. %)
  • Oligomer M3 ⁇ is an Oligomer.
  • the ingredients combined to make Oligomer M3 include the following:
  • Oligomer M3 Material description Wt. % TDI Type ll 21.26 BHT Food Grade 0.05 2-HEA 14.18 Dibutyltin Dilaurate 0.05 Pluracol P1010 64.46 Total (due to rounding of significant 100.00 figures may be +/ ⁇ 0.10 wt. %)

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