TW200401912A - Methods for making and using point lump-free compositions and products coated with point lump-free compositions - Google Patents

Abstract

A method is provided to manufacture a coated substrate, such as an optical fiber, without undesirable point lumps. The method filters a coating composition while controlling the filtering temperature, pressure drop across a filtering assembly, and filter pore size to achieve a resulting filtration factor not greater than 250,000 s-1. The filtration factor is a function of filtering temperature and pressure drop across the filtering assembly. Typically, the coating composition is filtered by passing the coating composition through one or more filters of the filtering assembly, having an absolute pore size rating in the range from approximately 0.05 to approximately 5 microns, at a temperature less than approximately 105 DEG F (40 DEG C), and at a pressure drop Δ P across the filtering assembly of at most approximately 80 psig, wherein the ratio of pressure drop (mPa) to viscosity (mPa.s), which is dependent upon filtering temperature, minimizes the filtration factor to ≤ 250,000 s-1.

Description

200401912 发明 Description of the Invention: This case claims the priority of the US Provisional Application No. 60 / 378,663, dated May 9, 2002, which is incorporated herein by reference. [Technical Field to which the Invention belongs]

The present invention relates to a technique for coatings for products that require a substantially clear surface. Specifically, the present invention is a solution to the problem of dot-like bumps in (for example, optical fiber) coatings. In the filtering process of the coating, the filtering conditions such as pore size, ® force difference ( pressure drop) and temperature. [Prior art]

Optical fibers used for light transmission are exceptionally strong when stretched and have very few internal defects. However, even a small surface flaw can make the fiber brittle and easily damaged. Therefore, these optical fibers are generally covered with one of the main and non-essential protections disclosed in Shustack U.S. Patent Nos. 6,014,488, 5,352,712, 5,527,835, 5,538,791, 5,587,403 and 6,048,911 Secondary coating. All of these patents are incorporated herein by reference. In the manufacture of fiber optic cables, a pre-formed glass rod (which is typically manufactured in a separate process) is suspended vertically and moved into a heating furnace at a controlled speed. The pre-formed glass rod is softened in a heating furnace and at the melting end of the pre-formed glass rod is stretched freely 6 by a capstan at the base of a draw tower to form a optical fiber. To protect stretched fibers from damage caused by abrasion or handling, the fibers have traditionally been protected by a coating. This coating is applied to the optical fiber before it reaches any rolling machine or capstan to limit any defects that may occur during its winding. In addition to protecting only the surface of the fiber from abrasion, the coating's junction system is selected to limit transmission defects. Specifically, substandard coatings such as those described in U.S. Patent No. 4,962,992 to Chapin et al. (All incorporated herein by reference) can cause large bubbles, voids, non-concentric coatings, and Microbending, each of these often causes transfer defects. Optical fibers with double coatings are generally used for cables to achieve the designed flexibility and improved performance while protecting against the aforementioned undesired effects. Generally speaking, a double-coated fiber includes a coating system, which has an internal or primary coating. The coating is characterized by a relatively low modulus elasticity. A rubbery material is coated on the optical fiber. The primary coating should effectively reduce the stress transmitted to the glass by external lateral forces, thus reducing the micro-bending of the glass. Primary coating materials are characterized by having an equilibrium modulus of elasticity in the range of about 50 psi to about 200 psi. The equilibrium modulus can be defined as the final modulus that reaches the cross-linked material in time or at high temperature. This modulus is chosen so that the primary coating achieves its primary purpose (that is, the stress attenuation and uniform distribution applied to the fiber). Through this attenuation and distribution, the loss caused by the micro-bend will be substantially reduced. The purpose of the main coating is to allow a limited degree of bending without causing microbending aattenuation error ° Although the edge coating does not directly participate in the role of the signal transmitted through the fiberglass, the coating is The performance of light is critical. This coating is used to provide (1) the strength i maintenance (strength retenti〇n); (2) environmental protection; (3) 杬 micro examination of phase loss, and (sentence to help fiber consistency; and when the bundle into a cable In the structure, separate independent optical fibers. The main coating is usually soft or elastic. Because the main coating has a low glass transition temperature (glass transiHon temperatUre) (such as -2 (TC To -50.〇, it has a low modulus and has the function of absorption. The main coating also has #good adhesion to glass in various environments and twisting conditions, and Tongri Temple is sufficiently low The adhesiveness can easily peel off the coating and has delamination resistance. This strippabiiity is described in US Patent No. 6,014,488 issued to Shustack, all hereby incorporated For reference, an outer layer or a secondary coating is applied over the primary coating. The secondary coating is usually a high modulus material used to provide abrasion resistance and low friction to the coated optical fiber. The dual coating material uses the main coating to provide buffer for the optical fiber. It acts and disperses external forces with the secondary coating, thereby preventing the optical fiber from being bent. The secondary coating is generally a hard, scratch-resistant coating whose glass transition temperature may be equal to or higher than About 80 ° C. The secondary coating is specifically selected to have high modulus and low ductility and to protect against environments such as harsh mechanical and chemical conditions. The coefficient of friction must not be too low (slip the fiber) or Too high (tackiness or stickiness). It is also desirable to maintain a proper degree of cure which has limited the coating's slip and tackiness. Generally speaking, the primary and secondary coating systems are Cured with ultraviolet light (cross-linked). However, other curing techniques include electron beam or electromagnetic radiation including heat and visible light. Typical coated optical fibers have a total diameter of about 245 μιη. The stretched glass fiber core— Generally has a diameter of about 8 μm, and has a concentric cladding of about 117 μm. The thickness of the main coating is about 65 μm, and the outer layer is coated with the 55 μm Form the balance of the thickness of the coated light. The innermost structure or glass fiber is designed to carry the signal from one station to another. Generally doped with germanium and / or erbium The glass core is surrounded by a cover layer derived from pure glass. The refractive index of the glass core is greater than the refractive index of the cover layer. This ensures that the signal is focused and limits the beam to the center of the core. The UV-curable fiber The coating system generally includes an oligomer, a monomer, a photoinitiator and additives. Typical oligomers, monomers, photoinitiators and additives are disclosed in U.S. Patent No. 6,014,488 issued to Shustack and Patent No. 5,352,712, all incorporated herein by reference. The oligomer has a high viscosity and provides the basic properties of the coating, while the low-viscosity monomer helps to adjust the cross-link density or to help adjust the viscosity. The photo-initiator is used to initiate the curing reaction, and the additive system includes modification properties such as adhesiveness (such as Shixi bonding agent), storage stability (such as storage time), and friction coefficient. The glass portion of the optical fiber is conventionally manufactured via a stretching table. A consolidated blank or preform is put into a heating furnace set between 1900 ° C and 2300 ° C, and a high-precision computer-controlled execution system is used. The optical fiber is drawn with a preform from the molten glass. The bare fiber was cooled down to 50 ° C-60 ° C as it was passed down to the station. The coating is applied to the bare optical fiber and it is stretched at about 35 ° C to 40 ° C for a stretching speed of more than 800 meters / minute. For higher speeds, more adjustments need to be made to the viscosity of the coating. The coating can be applied in a traditional "wet-on-dry" process. In the wet stack dry process, the uncured primary coating is applied to the bare fiber. The primary coating is then at least partially cured via a set of ultraviolet lamps. Once this curing occurs, the secondary coating is applied and cured by another set of UV lamps. The secondary coating was applied to the "dry" primary coating in a "wet" state. 200401912

In addition to the wet-on-wet process, there is also a wet-on-wet process. In a wet-on-wet process, the primary coating is applied before the secondary coating. However, the primary coating was not cured before the secondary coating was applied. Therefore, both coatings are cured simultaneously. The special design of such a coating device for a wet-on-wet process is described in U.S. Patent No. 4,474,830 issued to Taylor, which is incorporated herein by reference in its entirety. Because only a single set of UV lamps are to be used in wet-on-wet applications, a smaller stage than a wet-on-dry process can be used and performed at a faster rate. Traditionally, the coating composition is filtered before being coated with the glass fiber. Use, for example, a nylon filter with a pore size of 0.1-5.0 μm at a temperature of about 105 ° F (40 ° C) and a pressure difference (Δρ) of about 40 psig (275 kPa) to about 60 psig (415 kPa) ).

However, even with this filtering step, the coated optical fiber still has a defective coating. Generally speaking, the imperfections of the coating are due to defects in the manufacturing process (that is, the process used to coat the glass fiber) or compositions (that is, the materials and compositions that form the coating )defect. Process defects include, for example, concentricity, while composition defects include, for example, fiber content or other contaminants. In addition, for example, a bubble or delamination defect may be a process defect, a composition defect, or both. One of the defects in the composition is a point lump. The characteristics of this stippled bump are known. However, the inventors believe that the cause of the dot-like bumps is the high molecular weight fragments (hereinafter referred to as gels or gel compositions) of gel formations 11 200401912 of the secondary paint .

Dotted bumps can cause (1) the coated fiber to exhibit low tensile modulus, mainly due to mechanical obstructions in the post-stretch process (such as ink coloring), or (2) the coating on Defects that cause microbending or attenuation. These gel compositions may be visually perceptible or may require magnification. However, most of the point-like bumps caused a shift of the entire fiber diameter of 5 μm (or about 2% of the total diameter). In addition, although the appearance of dot-like bumps does not necessarily reduce the tensile strength of the coated optical fiber, the dot-like bumps may become stuck in the subsequent dyeing step.

The spot-shaped bumps often have the same refractive index as the cured coating. So although they are different, they are formed from the same material. Figure 1 illustrates an optical fiber 10 without any point-like bumps. It has a glass fiber 112, a primary coating 114, and a secondary coating 116. A dot-like bump (an external dot-like bump) causes the total diameter of the coated fiber to change. The outer dot-like projection 128 (shown in Figure 2) is generally visible because, although the refractive index of the projection is the same as that of the coating, at least the bulge is observable. Fig. 2 illustrates a portion of an optical fiber 120 having glass fibers 122, a primary coating 124 and a secondary coating 126, and an external dot-like projection 128. Figure 3 illustrates a portion of an optical fiber 130 having glass fibers 132, a primary coating 134 and a secondary coating 136, and an internal dot-shaped projection 138. Internal stippled bumps are often invisible to the naked eye. The internal point-like bumps usually cause the compression of the main coating 12 200401912 (compression) so that the diameter of the coated optical fiber does not change and only the relative diameter of the individual component is changed. The appearance of point bumps is a difficult problem. Due to the competitive nature of the fiber optic industry, it is not economical to single out or eliminate fiber optic products containing such defects. In earlier fiber optic technologies, the cost of producing coated optical fibers was much higher than today, so the cost of identifying defective products was not sufficient. This problem is aggravated because the dot-like bumps cannot be detected until the coating is applied to the glass fiber. Adding to the difficulty of avoiding the inclusion of punctiform bumps is the test. Unfortunately, the only known method for testing the spotted bumps is to stretch the fiber from a preform and coat the stretched fiber. The appearance of the dot-like bumps can be detected only after the coating is applied to the glass fiber. Even then, no known automatic test device was developed to separate the spot-shaped bumps. However, some devices do require the occurrence of specific conditions to determine the total number of defects, but cannot specifically determine the number of point bumps. Therefore, the only known method for determining point bumps on coated light is to manually and scan the surface with a microscope and count. Therefore, this testing process is time consuming and expensive. It is known to filter uncured secondary coating materials in a coating manufacturing facility. However, this is done under high pressure to speed up production and remove tiny (still visible) particles. This filtration method does not remove any invisible gels (which are believed to be the source of spotted bumps). In addition, the same type of problem (that is, the inclusion of punctiform bumps) is known to cause the same undesirability on other products that require coating (such as compact disks, dental compositions, and layered surfaces). Point-like bumps. Therefore, there is a need in this field to provide a method for economically manufacturing an optical fiber by removing the gel or gel composition in the coating before coating the bare optical fiber so that its coating has few or no spots Bump defect.

[Summary of the Invention] According to the discovery of the characteristics of point bumps in a coating made of a liquid material (as opposed to a gaseous or solid coating material), the present invention removes the point bumps to find solutions to the point bumps Problem approach.

Therefore, the "spotted bump" used throughout the specification and the scope of the patent application is an object in the coating and composed of a material different from the material of the coating. The stippled bumps may be visible (to the naked eye), visible through magnification, or invisible when they have the same refractive index as the secondary coating. Pointed bumps will cause one or more of the following: (1) low tensile force in the coated optical fiber; (2) microbending or attenuation due to defects in the coating; and ( 3) Visible (by the naked eye or by magnification) perturbation of the coated fiber diameter. In order to avoid the occurrence of spotted bumps or to minimize the occurrence rate of spotted bumps on the optical fiber coating, specific conditions are selected to filter the coating composition. Specifically, it was found that selecting a suitable pressure difference (ΔP) across at least one filter medium in the filter device, the temperature of the filter uncured coating material 14 200401912 degrees, and the hole size of the filter can make the dot-like protrusions The occurrence of blocks is minimized or eliminated. These factors are specifically selected so that a filtration factor determined by Δρ and the filtration temperature is less than or equal to 250,000 s-1 in the filter medium of at least one filter device. This process is used to pass through the material used to form a coating on a substrate (such as the material used as a secondary coating for optical fibers, the material used to form a coating on an optical medium, such as a pocket magnet Disks or digital video disks, dental applications or laminated surfaces). In this specification, the filter coefficient (γ) of the filter media of all filter devices is defined by the following formula: AP (mPa) / _κ η {ηιΡα ^) = Ύ {8} ⑴ where ΔP is across the filter device The pressure difference between the individual filter media and the viscosity of the individual filter media of the coating composition in the filter device. This process can be used to filter secondary coatings for a wet-on-wet or wet-on-fiber coating process. Preferably, the process can be used for filtering, and as a secondary coating for a wet-on-fiber optical fiber coating process. The present invention selects an appropriate temperature, pressure difference, and filter pore size to remove gel particles that would cause spot-like bumps. Specifically, the coating composition is passed through a filter having a hole size from about 0.05 μm to about 5 μm, at a temperature of 15 200401912 degrees less than about 105T (4 (rc), and across a single or Is a multiple filter media with a pressure difference of about 0 to about 5 psig 'wherein the ratio of the pressure difference (mpa) to viscosity (mPa-s) will use a filter with a pore size from about 0.05 μm to about 5 μm The filter coefficient is reduced to 2 250,000s · 1. It should be noted that the natural logarithm of the viscosity is shown to be directly proportional to the temperature. Therefore, the spotted bumps can be removed by filtering the coating composition by the method according to the present invention. (Ie, interferences visible in the primary or secondary coating) 'or any invisible deformation that causes microbends, attenuation, or reduction in fiber strength. Other objects, features, and advantages of the present invention will be in The following detailed description of the preferred embodiment is more obvious in conjunction with the accompanying drawings (where similar numbers are used to indicate corresponding parts in several figures). [Embodiment] A. Point-shaped protrusions Figure 1 Figure 1 does not have any points The optical fiber 11 is shaped like a bump. The center of the optical fiber 110 is a glass fiber 112 surrounded by a primary coating 114 and a secondary coating 116. Referring to FIG. 2, a one-point bump 128 is a secondary coating. An interference on or in 126. Basically, the dot-shaped protrusion 128 is a defect when a coating is applied on a glass fiber surface, which causes the female to 126 dislocation. The cause The misalignment of the dot-shaped bumps 128 will cause the surface of the secondary coating 126 to shift about 5 μm compared to the position without the dot-shaped bumps 128. 16 200401912

As shown in Fig. 2, the external interference caused by the external dot-like projection 128 is a displacement extending from the secondary coating layer 126 in a direction away from the primary coating layer 124 and the glass fiber 122. FIG. 3 illustrates an internal dot-like projection 138 which is displaced by the secondary coating 136 extending in the direction of the primary coating 134 and the glass fiber 132. Although the figure is not drawn to scale, the total displacement of any membranes or transitions with dot-like bumps 128, 138 compared to optical fibers without dot-like bumps is about 5 μm. In some cases, the dot-like protrusions 128, 138 may be smaller, causing a displacement of about 3 μm. In other cases, the measured displacement may be about 2% of the total profile of the fiber. Of course, a single point-like protrusion 148 can form both internal and external influences (Figure 4).

When the internal dot-shaped protrusion 138 appears, it may not be detected from the surface of the optical fiber 130. The in-phase extension of the interfering phase formed by the internal dot-like projections 138 will force the primary coating to leave its original position. Because the composition of the primary coating 134 is flexible and forced to leave its original position, the primary coating 134 is easily compressed to make room. When the internal dot-like projections 138 appear, the transition bands of the primary coating 134 and the secondary coating 136 are removed, for example, about 5 μm, but the displacement may be seen only when the light is refracted, other times It cannot be seen from the surface of the optical fiber 130. However, this feature is often seen in a scanning electron microscope or possibly a standard stereo microscope at a magnification of about 200 times. 17 The method of the present invention is specifically designed to remove the point-like projections 128, 138, 148 in an optical fiber 120, 130, 140. The appearance of the dot-shaped protrusions 128, 138, and 148 may cause the coated optical fiber to have low tensile force, attenuate signal loss, or easily have a dirty surface. B. Method for manufacturing optical fiber

Fig. 5 is a diagram illustrating a process of manufacturing a coated glass fiber. In this process, a pre-formed glass material is provided (step 162) and a draw tower is provided to draw a bare glass fiber therefrom (step 164). The bare drawn glass fiber is reactive and also damaged. It is therefore important to complete the coating formation step before operation. Therefore, in a preferred wet-on-wet coating process, the primary coating is provided (step 160) and applied to the bare drawn glass fiber (step 166). Either simultaneously or immediately after this step, a secondary coating composition is provided (step 161) and applied to the primary coating (step 168). Using a set of UV lamps, the two coatings are cured in situ simultaneously (step 170). Although such wet-on-wet applications are preferred, it is still possible to apply the secondary coating after the primary coating is at least partially cured. Finally, a capstan is used to pull out from the stretching table and roll the coated optical fiber into a roll (step 172). Further, as mentioned above, it is also within the scope of the present invention to exclude the primary coating as a whole and to use only a single coating. Generally, the primary and secondary coating compositions are prepared away from the locations where they are commercially applied to the glass fibers. It is of course preferred that the 18 200401912 primary and secondary coating compositions can be manufactured and filtered where they are commercially applied to the glass fiber. Figure 6 illustrates a typical step for preparing a secondary coating that includes mixing the secondary coating ingredients to form a mixture (step 182), cooling the mixture (step 183), and then filtering the cooled mixture ( Step 184) The secondary coating composition is formed.

The mixing of the minor coating ingredients typically occurs at an elevated temperature (e.g., about 140 ° F (60 ° C)) to facilitate mixing and flow the ingredients. However, traditionally the hot mixture was cooled to 105 ° F (40.5 ° C) and then filtered at that temperature. The preparation of a primary coating composition also typically involves mixing its ingredients at a higher temperature to form a mixture, cooling the mixture to a temperature suitable for filtration, and then filtering the mixture to form the primary coating composition. The filtering process can be performed in a single stage, as shown in Figure 6, or divided into multiple stages. Steps 182, 183, and 184 are usually performed in a first position, where the filtered coating composition is prepared and placed into a container. The container of the coating composition is transported to a second position for coating the glass fiber. The present invention differs from the conventional process in that it uses unique filtering conditions to accidentally remove point bumps. This condition is explained below. C. Filtration of the secondary coating. Traditional filtration is performed by a nylon filter with a hole size of 0.45 μm. The pressure difference is between 40-60 psig and a temperature of 105 ° F. In contrast, the present invention reduces one or more conventional conditions to reduce the number of punctiform bumps of 19 200401912 or remove the final product. The present invention balances the filtering temperature, the pressure difference across at least one tearing medium across a filtering device, and the coefficient of the hole size of the filter to thereby obtain less than or equal to 250,000 in the filtering medium of the filtering device, preferably The filter coefficient is less than 100,000, more preferably less than 50000 s 1 ′, such as less than 43000 s-1. The thickness of the filter and media may also be a parameter, because thicker filters can have larger pore sizes than thinner filters and can also be very efficient. However, the pressure difference parameter takes into account the hole size and thickness characteristics. Under standard operating conditions, thicker media will have a larger pressure difference than thinner filter media with the same hole size. As shown above, the filter coefficient (γ) is defined by the following general formula I: ^ P {mPa) /-"^ T) = Y (S} ⑴ where ΔP is the pressure difference, and" is the coating composition The viscosity of the material passing through the individual filter media in the filter device. Therefore, the filter coefficient is calculated for each filter assembly of the overall filter device and the filter coefficient is determined so that at least one filter assembly in the overall filter device has The appropriate filter factor. Generally speaking, the filter assembly includes a support such as an enclosure or a housing, which contains a single filter medium or multiple filter media in parallel such that the AP system is the The pressure difference between the inlet 20 200401912 of the support and the outlet of the support. For example, the filter assembly may include a housing having one or more independent filter media disposed in parallel therein. It is also within the scope of the present invention. A filter device with a single filter medium can be used, especially a single filter, the device is arranged in a single housing. Within the scope of the present invention, a plurality of consecutive settings can also be used Filters, media, especially a plurality of filter housings containing filter media, wherein the housings are arranged in a continuous manner. Within the scope of the present invention, the filtering device may also include parallel and continuous housings. Preferably, All components pass through at least one filter medium that meets the desired filter and coefficient. For example, if the filter device has three shells, the first and second parallel shells each contain three parallel 5 and Pass the medium and feed the third housing with a single medium, and then the parallel housing (and its individual medium) all have the desired filter factor or the third housing (and its individual Medium) has the desired filter coefficient. Although not wishing to be bound by any theory, the spot-like bumps are presumed to be formed of a gel composition in a secondary coating before the glass fiber is applied to the glass fiber. It is believed that The elevated temperature causes the gel composition to partially dissolve or deform, and increased pressure gives the gel composition a partial dissolution or dissolution.幵 7 Extra "boost" to pass through the narrow hole size. Therefore, reducing the temperature and pressure will reduce the filtration coefficient and avoid the gel, and the product will be flexible enough to pass through the narrow hole. 21 200401912 The filter factor 'in this case' can be defined as the ratio of the pressure difference (ΔP) and the viscosity of the net material. The natural logarithm of the viscosity is directly proportional to the temperature of the fiber coating material. As mentioned earlier, The main factor in removing spotted bumps by filtration is the temperature at which the filtration is performed. If using conventional 105T, it must be balanced with a non-traditional low pressure difference across the filter. It has also been found that high temperatures can cause the coating to stick Degradation of the agent. However, the temperature is preferably lower than the traditional temperature. Generally speaking, the filtration is performed at a temperature of less than about 120T, such as between 50T and 120T, or between 70T and 105T. The preferred filtration temperature range is from 60T to 95 ° F (15.5 ° C to 32 2 ° C), and more preferably from 70 ° F to 90 ° F (21.2 ° C to 32.2 ° or even 70 °). F to 80T (21.2 ° C to 26.7 °. Although the data obtained show that lowering the filtration temperature has a positive effect on the properties of the point bumps, this effect is limited. It is believed that lowering the temperature too much (for example, low (At about 50 T) will cause the secondary coating to crystallize during filtration. Although lowering the temperature will limit the formation of stippled bumps on the final coated fiber, the coating solution before coating on bare glass fibers The formation of crystals in the solution also adds other problems. In addition, at lower temperatures, the time required to complete any filtration step becomes longer due to the increase in viscosity. At standard temperatures (eg 105 F) A typical flow rate through a standard 30-inch filter cartridge is about 100 grams per minute through a 10-inch filter (using a catridge filter). However, the temperature is reduced to 70 ° F Will be after 22 200401912

The filtration reduces the flow rate from a factor of 4 to 1. This is due to an increase in the viscosity of the coating due to a decrease in temperature. In fact, the secondary coating material and / or its individual ingredients are typically heated to 140 ° F to allow adequate extraction and mixing before filtering. The secondary coating material is then cooled before filtering. When the filtration system is performed at a temperature much lower than the standard 105 ° F, additional cooling is required between extraction / mixing and filtration, increasing the cost and time for manufacturing the coating solution. Therefore, when filtering at a lower temperature in the scope of the present invention, it is necessary to increase the surface flow through the area of the filter itself or the entire area of the filter device (such as an additional filter box or a larger filter surface area) To achieve the same flow rate as at higher temperatures.

In the filter coefficient formula I, AP is the pressure difference across the individual filter media in the filter device. The highest limit of the range of conventional APs is about 80 psig, such as between about 3 and about 40 psig. The pressure difference AP across individual filter media in the filter device usable in the present invention is from about 0 to 80 psig, 0 to 60 psig, or 5 to 60 psig, or 10 to 60 psig. However, the higher pressure difference in the use range is balanced by an unconventionally low filtration temperature. Therefore, the ratio of the pressure difference (mPa) to the viscosity (mPa-s) is controlled to reduce the filter coefficient to $ 25000 (^ 4. Preferably, the ΔP is from 35 to 55 psig, more preferably from 40 Up to 50 psig. Keeping ΔP at 40 psig and filtering at 70 ° F (making a filtration factor of about 43000 s' is effective when using a variety of hole size filters. It should be understood that the above-mentioned filtration factors can be used for a variety of Different types of filters and filtration systems. The aforementioned minimum filtration coefficient is known to include the system where the area of the filter is increased to allow use at low pressures. The aforementioned filtration coefficients indicate coatings with different viscosities, when Coatings with high viscosity can be performed at high temperatures and show the desired filtration coefficient. In the present invention, the standard ratio of the pore size of the filter is in the range of up to about 10 μηι, for example, from about 0.05 to about μιη, or from about 0.45 to about 3 μηι, from about 0.05 to about 5 μηι, or from about 0.1 to about 3 μηι. Within the scope of the present invention, one having an absolute rating (absol A filter with a pore size of ute rating), the pore size is in a range with a maximum limit of about 10 μηι, for example, from about 0.05 to about 10 μηι, or from about 0.45 to about 3 μηι, From about 0.05 to about 5 μm, or 疋 from about 0.1 to about 3 μm. A nominal rating refers to a filter that will be removed at least after a single pass (Equal to or greater than) 50% of all particles. An absolute rating means that a filter will remove at least (equal to or greater than) 99% of all particles after a single pass. Membrane filter hole size It is known that it is also the average pore size, and the range is from about 0.05 to about 0.6 μm, preferably 0 to 4 μm. The range of the hole size of the preferred membrane filter is from 0.1 μm to 0. · 45μηι. A typical membrane filter is a nylon membrane filter with a hole size of 0.45μm or a polytetrafluoroethylene 24 200401912 (polytetrafluoroethylene, PTFE) membrane filter with a hole size of 0. The central filter ( depth filter) The pore size, for example, is measured by a "bubble test" (see US Patent No. 5,468,382), and preferably ranges from about 1 to about 4. The preferred size of the pore size of the central filter The range is from 1 μm to 3.0 μm. _ Typical central filters are polypropylene central filters with a hole size of 3.0 μm. Membrane filters, filters, and central filters are known in this field. . Brother 7 and Brother 8 are respectively not used in a conventional membrane filter and a central filter of the present invention. Conventional central filters and membrane filters can be used in the filtration step of the present invention. Typical filters appear and are described in U.S. Patent No. 5,279,731 issued to Cook et al., U.S. Patent No. 5,468,382 issued to Ohtani, and U.S. Patent No. 5,864,421 issued to Cok et al. All of these patents are incorporated herein by reference. Figure 7 is a partial cutaway view of a conventional membrane filter used in accordance with the present invention, which appears and is described in U.S. Patent No. 5,864,421. Specifically, FIG. 7 is a diagram showing a general pleated film cassette filter. A filter membrane 203 is pleated when sandwiched between two liquid-permeable sheets 202 and 204 and is wound around a core with a plurality of liquid collection ports 205 on. A peripheral shield 201 is provided outside the filter film 203 to protect the filter film 25 200401912 film 203. The precision filter sheet film 203 is male-sealed at the opposite ends of the cylindrical object with a terminal disc 206. The end disc 2⑽ is connected to a seal portion of a filter housing (not shown) with a gasket 207 (gaSket). The filtered liquid system flows from an outlet 208 from the liquid collecting port of the core. Figure 8 illustrates a cross-sectional view of a conventional central filter that can be used in the present invention, instead of or in combination with the membrane filter of Figure 7. Such a central filter appears and is described in U.S. Patent No. 5,468,382. The central filter device includes a substantially cylindrical central filter medium 31 with a pleat 311. Each fold 311 extends along the length of the filter medium and the folds together extend parallel to each other around the filter. An inner support core 312 is disposed in the cylindrical central filter medium and contacts the inner pleats. An outer support cage 313 contacts the outer fold. A cylinder of the central filter medium may be a continuous sleeve without any sealed filter medium at the edges. A second possibility is to form the cylindrical filter medium 310 from a flat sheet of central filter medium, which has a seal to form the cylinder. A third possibility is to roll a flat rectangular sheet into a cylindrical cylinder, with two opposite edges of the sheet overlapping at least once. The transponder medium can also be a fibrous structure such as a polyhydrocarbon, a polyester, a polyurethane, a glass fiber, or a metal fiber. For example, the central transition element can be formed by a "refining and blowing process" (meh blowing 26 200401912 process) and its diameter is from ι_20 μηι, preferably 1-12 μηι. As mentioned above, the filtering step 184 (Fig. 6) can be a single stage or a series of stages. In one embodiment, step 184 is performed with a first filter or a pre-filter, which has a substantially larger hole size. Because the filter has a limited useful life, its cost increases as the hole size of the filter decreases. Therefore using a pre-filter with a larger pore size removes many large filtrates from the coating solution before using a relatively more expensive filter (with a smaller pore size). The final filter generally falls within the aforementioned pore size range. In all the descriptions, it should be noted that when referring to a filter device, it is also possible to use multiple filter media, and vice versa. In addition, adjusting the filtering characteristics, such as increasing the surface area will affect the calculation of the filtering coefficient, and increasing the surface area will reduce the resulting pressure difference. In addition, as described above, the surface area of the booster σ can achieve a low pressure difference, which is also within the range of this Maoming. However, the measurement of the pressure difference is measured across each filter, the assembly is' whether the filter, the assembly is a single-filter, H with a large or i surface area, or is arranged in a continuous and parallel arrangement. Multiple filters and filters. That is, the pressure difference is measured across each independent filter assembly, and has nothing to do with any other job assembly or device outside the filter, device. For example, a typical filter pack would be used to pump the coating composition from a supplemental tank and send it to a first k / filter. In this example, 27 200401912, it is assumed that the pump feeds the coating composition to the first filter at 40 psig. After the first filter, the coating composition flows into a first filter. However, according to the present invention, the pressure difference is measured across each independent filter assembly and is therefore not affected by external devices, upstream or downstream of the filter, such as pumps or heat exchangers. The integrated device used in the present invention may also include one or more pressure gradient devices provided between the inlet and the first filter and the last filtered outlet, such as a heat exchanger, a pump, or Valves before, after, or between independent filters will not affect the calculation of the pressure difference. The temperature is the temperature of the composition of the individual filter assembly. According to the outline of the foregoing steps, it is possible to limit the dot-like bumps that appear on a coating on a substrate (such as a coating on an optical fiber). The coating composition produced by the aforementioned method is used to form a cured coating having substantially no stippled bumps. For example, when measured by the following process, 0 to 0.001%, preferably 0 to 0.0001% of the coating is applied. The surface of the layer has spot-shaped bumps. For example, the aforementioned method can produce an optical fiber with an average of 0 to 10 dot-shaped dog blocks per kilometer, preferably from 0 to 5 dot-shaped bumps per kilometer, and more preferably from 0 to 2 dot-shaped bumps per kilometer. Piece. Therefore, the method of the present invention can be used to ensure that a batch of coating after filtration can make the coated optical fiber have an average of less than 10, generally less than 5, less than 2 or 0 point bumps per kilometer. The invention achieves a scrap rate that is much lower than conventional processes. In the industrial-grade manufacturing of the coating material according to the present invention, generally 28 200401912 includes continuous products or multiple batches of production every 12 consecutive months. 5 (M_ mock 'e.g. 50 (M_ 0ton)' It is proved that the coating composition is suitable for continuous production of less than about 10, less than about 5, or about 0 point bumps per kilometer. For example, the batch of suitable products makes At least 98% of the optical fiber coated with the material of the present invention has less than about 10 dot-like bumps per kilometer, less than about 5 dot-like bumps, less than 2 dot-like bumps, or about 0 dots. Bumps. For example, 1000 kilometers of optical fiber, at most 20 kilometers with more than 10 dot-like bumps per mol. Preferably, at least 99% of the coated optical fibers have less than about 10 dots per kilometer. Bumps, less than about 5 dot-like bumps, less than 2 dot-like bumps, or about 0 dot-like bumps; or at least 99.75% of coated fibers have less than about 10 dots per kilometer Bulges, less than about 5 bulges, less than 2 bulges, or about 0 bulges; or 100% coated optical fibers Less than about 10 point bumps per kilometer, less than about 5 point bumps, less than 2 point bumps, or about 0 point bumps. Therefore, the final product is caused by the point bumps (Made of 50 tons of final composition) the elimination rate is at most about 2%, preferably at most about 1%, more preferably at most about 0.25%. The number of the dot-shaped protrusions can be applied to the main coating in the following manner: Both the layer and the secondary coating are applied to the glass fiber and cured to determine: 1. Visible placement of a defect on a wound fiber or a length of fiber. Fix the fiber to a light and look for the The bumps or small dots on the optical fiber 29 200401912. You can also feel the bump on the coated fiber surface to identify a bump. 2. Set a color camera (such as SONY's 3CCD) to pass 20 times (200 times). Magnification, although for some defects a higher magnification is required for objective microscopes (eg LECCIA DMRX).

3. Adjust the lighting technology including bright field of view and fiber rotation to make defects appear. It is important to align the fibers. 4. Note the characteristics of the magnification at which the defect is visible. A stippled bump can be pointed out by a gel-like component with a refractive index similar to that of the coating or by the aforementioned simple interferer without any visible inclusions. This process for judging point bumps can also be used for coating compositions coated on other substrates.

If necessary, the primary coating material can be filtered by the method described above for the secondary coating. D. Method for drawing optical fiber In the method of the present invention, bare glass fibers 112, 122, 132, and 142 are drawn from a molten pre-formed glass in a conventional manner, such as Nos. 5, 9, and 10 As shown in the figure, and is generally taught by U.S. Patent No. 4,913,859, all incorporated herein by reference. However, the specific method of forming the glass fibers 112, 122, 132, 142 is not an integral part of the present invention. Fig. 9 illustrates a device generally designated 20 and used to stretch an optical fiber 21 from a cylindrical preform 22 prepared in 2004200412 and then apply the optical fiber 21. The optical fiber 21 is formed by locally and symmetrically heating the preform 22, and the preform 22 has a diameter of about 17 mm and a length of about 60 cm at a temperature of 2000 ° C. When the preform 22 penetrates and passes through a heating furnace 23, the optical fiber 21 is drawn from the molten material.

As can be seen in Figure 9, the stretching system includes the heating furnace 23, wherein the preform 22 is stretched to the size of the optical fiber, and then the optical fiber 21 is pulled away from the heating belt. The diameter of the optical fiber 21 is tested by a device 24 immediately after the heating furnace 23 to input a control system. In the control system, the measured diameter is compared with a better value and a signal is output to roughly adjust the drawing speed so that the diameter of the optical fiber reaches the better value.

After measuring the diameter of the optical fiber 21, the coating material (including the primary coating and the secondary coating) is coated by a device 25, and other details are illustrated in Figure 10 and discussed below. Then, the coated optical fiber 21 passes a centering gauge 26, an ultraviolet light device 27 for curing the coating material, and a device for measuring the outer diameter of the coating, which is passed through a capstan ( capstan) 29 moves and coils for testing and inventory before subsequent operations or sales. In the process of making the fiber into ribbons, adding jacketing, connectorization, cabling, and using them, the preservation of the intrinsically high-strength fiber is very important. 31 200401912 Figure ii)-A typical embodiment of a coating applicator 62 is used to coat a moving fiber of a coating material containing a primary coating, that is, a secondary coating. The coating machine 62 has an axis 57 of the optical fiber system, and moves along the axis. The coating machine 62 is used to apply a non-single-layer primary coating and a secondary coating to an optical fiber 21.

The coating coater 62 (shown in detail in FIG. 10) includes a housing 65 having an alpha octagonal inlet 66, and a continuous increase of the optical fiber 21 is entered from the horn-shaped inlet 66. The herringbone-shaped inlet 66 is connected to a cylindrical passage 67 and has an opening to a first slot cavity 68. A lower portion 69 of one of the first slot cavities 68 has a conical shape and communicates with a cylindrical passage 70 having an opening in the one-to-one second slot cavity 71. A lower portion 72 of the second groove cavity 71 has a conical shape and communicates with a cylindrical passage 73.

The coater 62 is operated so that there is a pressure difference between the grooves 68 and 71 and the surrounding atmosphere having the chamber pressure is larger than the pressure in the groove. In a typical embodiment, the grooves 68 and 71 are connected to a vacuum source (not shown) along lines 76 and 77, respectively. Aligned with the cylindrical passages 67, 70, and 73 are first and second dies 81 and 82 having die openings 84 and 86, respectively. Each die opening 84 and 86 is defined by a wall or a land. "Die" herein refers to the portion of the coater 62 which finally defines or helps to limit the coating given around the optical fiber. It should be observed that in one embodiment, the mold openings 84 and 88 associated with the first and second molds, respectively, have a diameter that is substantially larger than the diameter of the channel 73 32 200401912. On the other hand, the diameter of the channels 67 and 70 may be larger or smaller than the diameter of the die opening. However, in a typical embodiment they are relatively small to restrict air inflow. Generally speaking, each of the openings 84 and 86 has a product having a diameter equal to about 1.5 and an outer diameter of the optical fiber.

In addition, the coating machine is provided to provide a flow path of two materials. Such disk-like flow channels appear in U.S. Patent No. 4,474,830 and U.S. Patent No. 4,512,944, all of which are incorporated herein by reference. The space between the surfaces (described therein) defines a flow channel 93 provided to a first coating material 94 which provides the fiber with a buffering layer 64. The flow channel 93 has a channel where at least one element is moved perpendicular to the optical fiber along the longitudinal axis 57. In a typical embodiment, the flow channel 93 is disk-shaped and perpendicular to a channel for moving the optical fiber. In addition, the thickness of the flow channel 93 in the direction parallel to the channel where the fiber is moved is relatively small, on the order of about 2-10 mils. The size of the void at the point adjacent to the point where the coating material is applied and parallel to the channel that moves the fiber along the longitudinal axis 57 is called its thickness and is generally less than three times the fiber diameter. Generally, the voids are less than twice the fiber diameter. In fact, all known or recently developed methods for providing a stretched bare glass fiber can be used in the method of the present invention. In addition, when a wet stack wet process is preferably used to apply a primary coating and a secondary coating to glass fiber, the wet stack dry coating process using the method of the present invention is within the scope of the present invention. 33 200401912 The present invention can be applied to any primary and secondary coating composition. Therefore, the specific composition of the primary and secondary coatings is not part of the invention. For completeness, however, the components of a typical primary and secondary coating are described below. E. Coating composition 1. Main coating

The main coatings used in the present invention can be in any form known in the art. However, a typical main coating can be formed from the following ingredients: (1) (meth) acrylate-terminated urethane oligomer terminated with methacrylate; (2) monomer diluent (3) Optional adhesion promoter; (4) Optional photoinitiator and (5) Stabilizer, such as the United States awarded to Shustack No. 6014488, which is incorporated herein by reference in its entirety. It is within the scope of the present invention to provide no primary coating, that is, to use only a single coating to protect the glass fibers. a. Oligomers The urethane oligomers whose methacrylate ends are selected to be capable of undergoing homopolymerization to form the main structure of the main coating layer 30. The component whose terminal end is an acrylate or a fluorenyl acrylate is a fully aliphatic urethane ethyl acrylate or a methacrylate oligomer. The urethane acrylate or methacrylate oligomer bag 34 200401912

The weight of the uncured main coating material (composition) is from about 10% to about 80% (based on the total weight of the composition). Preferably, the oligomer component comprises from about 15% to about 70%, more preferably from about 20% to about 60% by weight of the composition (based on the total weight of all the components). The urethane oligomer whose terminal is acrylate or methacrylate in the present invention is the product of the following reaction (i) an aliphatic polyol; (ii) —aliphatic Polyisocyanate; and (iii) an endcapping monomer that can provide a reactive end, the reactive end of which is acrylic acid or methacrylate.

However, it is the functional group backbond of the oligomer rather than the end group, which gives the composition good characteristics. Therefore, a similar system to the aforementioned acrylate-based or fluorenyl-based composition (but possessing any reactive terminal functionalities) meets this requirement equally. Therefore, the fluorenyl acrylate can be partially or completely replaced by terminal functional groups of various other examples (which can be reacted by irradiation or other methods (either induced by free radicals or cured by cations) to provide a coating that performs well. . These terminal functional groups include radical systems, such as thiolene systems (based on the reaction of polyfunctional thiols and unsaturated polyenes, unsaturated polyenes such as vinyl ether); ethylene Sulphide (vinyl su lfide); allylic ether (bicyclicene and bicyclicene)); amine-ene (amine-ene) system (with polyfunctional amines and unsaturated polyethers 35 200401912

Based on the reaction); acetylene system; the reactive part of the compound in the system is in the molecule rather than at the end; other ethylene (such as styrene) system; acrylamide system; allylic system An itacate system and a crotonate system; and a cationic curing system such as an onium salt-induced vinyl ether system and an epoxy-terminated system (which React by opening the ring); and any other compounds taught in US Patent No. 5,352,712 to Shustack, which is incorporated herein by reference in its entirety, possess a reactive end-based compound. It is foreseeable that virtually any terminal functional group does not adversely affect the desired properties of the cured composition (ie, oxidative, thermal, and hydrolytic stability and moisture resistance) when cured by irradiation or other methods. Compounds that can be used as the terminal coating monomer include, but are not limited to, acrylic acid, methacrylic acid, vinyl ether, vinyl su lfide, allylic ether, Bicyclicene, mercaptan, acetylene, epoxide, amine, styrene, acrylamide, and others. Suitable for use as a terminal-coated monomer, a compound having a hydroxyl group at the end includes, but is not limited to, hydroxyethyl acrylate; hydroxyethyl methacrylate; Hydroxypropyl acrylate; hydroxypropyl methacrylate; hydroxybutyl acrylate; hydrogen 36 200401912 hydroxybutyl methacrylate; dilute propylene Allyl ether; hydroxyethyl vinyl ether 6 | (hydroxyethyl vinyl ether); hydroxypropyl vinyl ether; hydroxybutyl vinyl ether; hydroxybutyl vinyl ether Hydroxyethyl mercaptan; hydroxypropyl mercaptan; hydroxyethyl-3_mercaptopropionate; and hydroxypropyl-3-hydrocarbylthio Propionic acid (hydroxypropyl-3-mercaptopropionate). Examples of the polyol (i) may include polyether polyol (polyol polyol); hydrocarbon polyol; hydrocarbon polyol; polycarbonate polyol; polyisocyanate polyol ( p〇lyis〇cyanate polyol); and mixtures thereof. The polyol should be limited or preferably not contain polyester or epoxy backbone. Polyether polyols are typically based on linear, branched, or cycloalkyl oxides, where the functional group of the alkyl group contains from about one to about twelve carbon atoms. Such polyether evening alcohols include, but are not limited to, polytetramethylene polyols, polymethylene oxides, polyethylene oxides, polyethylene oxides, Polypropylene oxide (polypropylene oxide), polybutylene oxide (polybutylene oxide), and isomers (isomer), and mixtures thereof. A polyether polyol may also contain at least some units of polytetramethylene oxide and / or polypropylene oxide. For longer-term stability, the oligomer component may contain a small amount of polyester-based aminoethyl acrylate, instead of containing only the above-mentioned oligomers of 37 200401912. Polyether polyols are typically based on linear, branched, or mesogenic oxides, where the functional group of the alkyl group contains from about to about one carbon atom. The polyol can be prepared by any method known in the art and can have a variety of average molecular weights (in this example, determined by ASTMD-3592 卩 vapor pressure osmometry), the polymer The average molecular weight of the ether polyol is sufficient to provide an overall oligofluorene based molecular weight of greater than about dalton. Examples of these polyether polyols include, but are not limited to, polytetmmethylene polyol (polytetmmethylene p〇ly〇1), polymethylene oxide (p〇iymethylene oxide), polyethylene oxide (p〇 丨 yethylene Oxide), polypropylene oxide, polybutylene oxide, and isomers thereof, and mixtures thereof. Representative hydrocarbon polyols that can be used include, but are not limited to, based on linear or branched hydrocarbon polymers (molecular weights from 600 to 4,000), which are, for example, fully or partially Hydrogenated polybutadiene; 2-polybutadiene hydrogenated to an iodine number from 9 to 21; and fully or partially hydrogenated polyisobutene. Representative hydrocarbon polyols include, but are not limited to, the reaction product of a dialkyl carbonate with a dilute diol (optionally copolymerized with an ene ether diol). The polyisocyanate component (ii) may be non-aromatic. Non-aromatic polyisocyanates of 4 to 20 carbon atoms can be used. Suitable saturated aliphatic polyisocyanates include, but are not limited to, isophorol diisocyanate (isopharone (iiis〇cyanate); -4,4'-diisocyanate); 1,4-tetramethyiene diisocyanate; 1,5-38 200401912

Pentamethylene diisocyanate (1,5-pentamethylene diisocyanate); 1,6-hexamethylene diisocyanate; 1,7-heptamethylene diisocyanate 6 purpose (l, 7-heptamethylene diisocyanate); 1,8-octamethylene diisocyanate; 1,9-ninemethylene diisocyanate (l, 9 -nonamethylene diisocyanate); 1,10-decamethylene diisocyanate; 2,2,4-trifluorenyl-1,5-pentamethylene diisocyanate (2, 2,4-trimethyl-l, 5-pentamethylene diisocyanate); 2,2-dimethyl-l, 5-pentamethylene diisocyanate); 3-methoxy-1,6-hexamethylene diisocyanate (3-methoxy-l, 6_hexamethylene diisocyanate); 3-butoxy_1,6_hexamethylene diisocyanate Purpose (3-butoxy-l, 6-hexamethylene diisocyanate); omega, omega'-dipropylether diisocyanate; 1,4-cyclohexyl diisocyanate (l, 4 -cyclohexyl diisocyanate); 1,3- Hexyl diisocyanate (l, 3-cyclohexyl diisocyanate); trimethylhexamethylene diisocyanate (trimethylhexamethylene diisocyanate); 1,3-bis (isocyanic acid) l, 3-bis (isocyanatomethyl) cyclohexane); 1,4-diisocyanato-g-butane; l-4-diisocyanato-butane; biuret of hexamethylene diisocyanate hexamethylene diisocyanate); dicycloheptyl diisocyanate methyl 2,5 (6) -bis (diisocyanate fluorenyl) bicyclo (2,2,1) (isocyanatomethyl) bicyclo (2,2,1) heptane) and mixtures thereof. Isophorone diisocyanates are possible aliphatic polyisocyanates. Suitable 39 aromatic polyisocyanates intentionally include toluene diisocyanate (toluene diisocyanate); ~ diphenylmethylene diisocyanate (diphenylmethylene diisocyanate); tetramethylxylene diisocyanate (tetramethyl) xylene diisocyanate); 1,3-bis (isocyanatomethyl) benzene; p, m-phenylene diisocyanate; 4 4,4'-phenylphenyl diisocyanate (4,4'-diphenylmethane diisocyanate); dianisidine diisocyanate (4,4 diisocyanate_3,3'_dimethoxy-1, Γ- diphenyl diisocyanate (4,4'_diisocyanato_3,3'-dimethoxy-l, l'-biphenyl diisocyanate)); dimethyl p-diaminobiphenyl diisocyanate S (tolidine diisocyanate ) (I.e. 4,4'-diisocyanato-3,3'-difluorenyl-1,1'-diphenyl diisocyanate (4,4'-diisocyanato-3,3'-dimethy-l, l'- biphenyl diisocyanate)); and mixtures thereof. The reaction rate between hydroxyl-terminated polyols and diisocyanates can be increased by using 100 to 200 ppm catalyst. Suitable catalysts include, but are not limited to, dibutyl tin dilaurate, dibutyl tin oxide, dibutyl tin di-2-hexoate, oleic acid Stannous oleate, stannous octoate, lead octoate, ferrous acetoacetate, and amines such as triethylamine, Diethylmethylamine, triethyldiamine, dimethylethylamine, morpholine, N-ethyl morpholine, Piperazine, nitrogen, nitrogen-dimethyl 200401912 N, N-dimethyl benzylamine, nitrogen, nitrogen-N-dimethyllauiylamine, and mixtures thereof. The terminal-coated monomer (iii) may be a compound which provides at least one reactive terminal and preferably provides an acrylate or methacrylate terminal. Suitable hydroxyl end-point compounds that can be used as terminal coating monomers include, but are not limited to, hydroxyl alkyl propionate or methacrylate. Similar to a compound system based on propionate, but with any reactive terminal g-energy group, it is equally suitable. A variety of other exemplified terminal functional groups may be reacted by irradiation or other methods (either induced by free radicals or cured by cations) to provide a well-performing coating that includes (but is not limited to) by a 'radical system such as sulfur Thiolene system (based on the reaction of polyfunctional thiols and unsaturated polyenes, such as vinyl ether; vinyl su lfide; allylic ether) Bicyclicene); amine_ene system (based on the reaction of polyfunctional amines and unsaturated polyenes); acetylene system; the reactive part of the compound in the system is in the molecule rather than at the end; other Ethylene (such as styrene) systems; acrylamide systems; aliylic systems; itacate systems and crotonate systems; and cationic curing systems (such as phosphonium salt-induced ethyl acetate) Dilute ether (onium salt-induced vinyl ether) system and epoxy-terminated system (which reacts by ring opening); and any other Compounds with a reactive end. Virtually any terminal functional group does not negatively affect the desired properties of the cured composition (ie, oxidative, thermal and hydrolytic stability, and moisture resistance) when cured by irradiation or other methods The impact is foreseeable. Similar systems are also disclosed in U.S. Patent No. 5,352,712 issued to Shustack as 41 200401912 and U.S. Patent No. 5,572,835, all of which are incorporated herein by reference. Typical Acrylates and Methacrylates Contains hydroxyethyl acrylate, hydr0Xyethyl methacrylate, hydroxypropyl acrylate, hydroxypropyl methacrylate methacrylate), hydroxybutyl acrylate, hydroxybutyl methacrylate, and so on.

The mole fraction of the polyol, diisocyanate, and terminal coating monomer may be about 1: 2: 2. b, New

The monomer dilution component compatible with the above oligomer is selected to prepare the main coating layer of the present invention and can react with the aforementioned oligomer. In this case, it should be reactive with the aforesaid agglomerates and each monomer has one or more acrylic or fluorenyl acrylic ester moieties. The monomer diluent can reduce the glass transition temperature Tg of the cured composition containing the monomer diluent, and can reduce the viscosity of the uncured (liquid) composition, making its viscosity at about 1000 to 25 ° C. In the range of about 10,000 cps, the monomer diluent comprises from about 10% to about 75% by weight of the uncured (liquid) composition based on the total (all ingredients) weight of the composition. For example, suitable monomer diluents include, but are not limited to, aromatic-containing monomers, such as phenoxyalkyi acrylate or methacrylate (such as phenoxyethyl (methyl) Acrylate); phenoxyalkalkoxy 42 200401912 alkoxylate acrylate or methacrylate (such as phenoxyethylethoxy (fluorenyl) acrylate or phenoxyethylpropoxy (methyl Base) acrylate); p-cumyl ethoxylated (meth) propanoic acid g purpose (pafa-cumylpheiiol ethoxylated (meth) acrylate); 3-propenyloxypropyl-2-nitro-phenylcarbamate Acid ester (3-acryloyloxypropyl-2-N-phenylcarbamate);

Or any monomer diluent known to adjust the refractive index of the composition contained therein. Compositions containing one or more of these are equally suitable. A monomer diluent that is disclosed later and described in Shustack US Patent No. 5,146,531 (herein incorporated by reference), for example, contains (1) an aromatic group; (2) —provides a reactivity (Such as acrylate or methacrylate) functional groups; and (3) -hydrocarbon groups.

Examples of aromatic monomer diluents that also include argon compounds and a vinyl functional group include, but are not limited to, polyalkylene glycol nonylphenylether acrylates such as polyethylene glycol Alcohol nonylphenyl ether acrylate or polyethylene glycol nonylphenylether acrylate; polypropylene glycol nonylphenyl ether acrylate; polyethylene glycol nonylphenyl ether methacrylate Polyalkylene glycol nonylphenylether methacrylates such as polyethylene glycol nonylphenylether methacrylate or polypropylene glycol nonylphenyl ether methacrylate 〇pyiene 43 200401912 glycol nonylphenylether methacrylate): and mixtures thereof. This single system is commercially available, for example, Toagasei Chemical Industry Co., Ltd. of Tokyo, Japan under the trade names ARONIX M110, Mill, M113, M114, and Ml 17, and Henkel Co. of Ambler, Pennsylvania, under the trade name PHOTOMER 4003.

Other suitable monomeric diluents further include linear or branched hydroxide alkyl acrylates or acrylates, the alkyl portion of which may contain eight to eighteen carbon atoms, such as hexadecanoic acid; Hexyl methacrylate; ethylhexyl acrylate; ethylhexyl methacrylate; isooctyl acrylate; isooctyl methacrylate; octyl acrylate; octyl methacrylate; decyl acrylate; methyl Decyl acrylate; isodecyl acrylate; isodecyl methacrylate; lauryl acrylate; lauryl methacrylate; tridecyl acrylate; tridecyl methacrylate; tetradecyl acrylate; Tetradecyl succinic acid methyl ester; palmityl succinic acid ester; palmityl methacrylate; octadecyl acrylate; octadecyl methacrylate; hexadecyl acrylate Hexyl vinegar; Hexadecyl methyl methacrylate; Dihydrocarbon diol esters of 14 to 15 carbons; Dimethacrylate 14 to 15 carbons Compound glycol esters; and mixtures of the foregoing. Cyclic monomers are also suitable, such as isobornyl acrylate; such as isobornyl acrylate; dicyclopentenyl acrylate; dicyclopentenyl methacrylate Purpose; feminine 44 200401912

Dicyclopentyl ethoxylate; dicyclopentenyl ethoxy methacrylate; propylene tetrahydrofurfuryl vinegar; fluorenyl acrylic acid tetrahydrofurfuryl ester; and mixtures thereof. Also suitable are TONE M-100 monomers, which are caprolactone monopropionate and are commercially available from Union Carbide, Danbury, Connecticut. GENORAD 1122 monomer is available from Commercially available from Hans Rahn, Zurich, Switzerland, which is 2-propanoic acid, 2- (((butyl) amino) hydrocarbyloxy) ethyl ester (2-(((butyl) amino) carbonyloxy) ethylester) and N-vinyl caprolactam 〇 A typical single system containing monomers with refractive index adjustment is disclosed here, either alone or with alkyl (meth) acrylate Combined, for example, lauryl acrylate. c. Adhesion promoter

An adhesion promoter may also be included in the main coating composition. Adhesion is a particularly important problem in high humidity and high temperature environments where the coating is easily delaminated from glass fibers. To provide protection in this environment, adhesion promoters are required. It is known in the art that the use of acid-functional materials or organofunctional silanes can improve the adhesion of the resin to glass. Silane is also a suitable adhesion promoter. In addition, in some environments, the use of adhesion promoters that have the function of bonding to the system during curing can help to release volatiles

Quality is minimized. Various suitable organic functional silanes include, but are not limited to, acrylate functional silanes; amine functional silanes; hydrogen thio functional silanes; acrylamide functional silanes; propylene functional silanes and vinyl functional silanes. The adhesion promoter may be substituted by methoxy or ethoxy. Useful organic functional silanes include, but are not limited to, mercaptoalkyl trialkoxy silane, (meth) acryloxyalkyl trialkoxy silane, and amine radicals. Aminoalkyl trialkoxy silane, mixtures thereof, and the like. Methacrylated silanes are preferred because they adhere well to the curing system. The hydrogen-sulfur functional group adhesion promoter also produces chemical bonds during curing and significantly reduces the curing speed of the system.

Other preferred organic functional silanes that increase adhesion in a humid environment include 3-acryloxypropyltrimethoxysilane, 3-acryloxypropyltrimethoxy silane, and 2-trioxoethoxylate (vinyl-tris (2-methoxyethoxysilane)), 3-methacryloxypropyltrimethoxy silane, 3-aminopropyltriethoxy silane ), 3-mercaptopropyl trimethoxy silane, 3-mercaptopropyl triethoxy silane, and mixtures thereof. The other adhesion promoter is 3-propenyloxypropyltrimethoxysilane. The silicon sintered component is added in a small but effective amount to form a shape after the curing 46 200401912 into the main coating composition to improve the adhesion of the composition to the surface of the substrate. The silane compound is about 0.01% to about 3% by weight based on the total weight of all the components. The silane compound may also be about 0.2% to about 2.0% by weight based on the total weight of all ingredients. d. Photoinitiator

The main component may also contain a photoinitiator. The necessity of this component is based on the envisaged curing mode. If the composition is cured by ultraviolet light, a photoinitiator is required. If the coating is cured by an electron beam, the photoinitiator can be removed. In UV curing examples, the photoinitiator (which promotes radiation curing with a small but effective amount) must provide a reasonable cure rate without causing premature gelation of the mixed ingredients. Suitable photoinitiators include (but are not limited to):

Hydroxycyclohexylphenyl ketone; hydroxymethyl-phenylpropanone; dimethoxyphenylacetophenone; 2-methyl-1_ (4- Methyl (thiol) phenyl) -2-morpholino-acetone-1 (2-methyl-l- (4-methyl (thio) phenyl) -2-morpholino-propanone-1); 1- (4- Isopropylphenyl) -2-ratoxy-2-fluorenylpropan-1--1- (1- (4-isopropylphenyl) -2-hydroxy-2-methylpropan-l-one), 1-(4- Dodecyl Basic Group) -2-Aerobic Oxygen-2-methylpropane-1-47 4701901912 (1 (4-dodecylphenyl) -2-hydroxy-2-methylpropan-l-one); 4- ( 2 Nitrooxyethoxy) phenyl- (2-pneumo-2-propyl) pyrene (4- (2-hydroxyethoxy) phenyl- (2-hydroxy-2-propyl) ketone); (Diethoxyacetophenone); 2,2-di-sec-butoxyacetophenone; diethoxy-phenyl acetophenone; and mixtures thereof.

A preferred type of photoinitiator is a phosphorus oxide, such as trimethylbenzoyldiphenyl-phosphine oxide (commercially available from the Chemical Division of BASF Corporation in Charlotte, North Carolina, Its trade name is LUCIRINTPO), trimethylbenzoylethoxyphenylphosphine oxide (commercially available from BASF, its trade name is LUCIRIN 8893) (trimethylbenzoylethoxyphenylphosphine oxide);醯) -2,4,4-trimethylpentyl phosphine oxide (bis- (2,6-dimethoxybenzoyl) -2,4,4-trimethylpentyl phosphine oxide), and bis- (2,4,6-trimethyloxy) Phenylhydrazone) -phenyl oxide scale (bis- (2,4,6-trimethylbenzoyl) -phenyl phosphine oxide) (trade name CGI 819) or bis- (2,6-dimethoxybenzidine) -2 Bis- (2,6-dimethoxybenzoyl) -2,4,4-trimethyl pentyl phosphine oxide (CGI 1700 or CGI 1800) is available from New York State Ardsley's Ciba specialty chemicals. The photoinitiator (when used) is preferably based on the weight of the total mixture 48 200401912 to about 0.5% to about 10% by weight of the uncured mixture. The amount of photoinitiator may be from about 1% to about 6%. The photoinitiator may be present in an amount to obtain a cure rate of less than 0.7 J / cm2 (measured as a curve of dose versus modulus). 2.Secondary coating

The secondary coatings used in the present invention may also be in any form known in the art. For example, a typical secondary coating is described in U.S. Patent No. 6,014,488 and U.S. Patent 5,327,712 issued to Shustack, all of which are incorporated herein by reference. The secondary coatings described therein include: (I) from about 10% to about 90% by weight of a fatty acid ethyl ester based on a polyester and / or polyether and including a reactive end Oligomers; (II) a viscosity adjusting component having a weight percentage of from about 20% to about 60% of a carbon hydroxide capable of reacting with the reactive end of (I);

(III) Non-essential, photoinitiators from about 0.05% to about 10% by weight, all of the above weight percentages are based on the total weight of (I), (II), and (III). The reactive end of the secondary coating may be a reactive end revealed to be suitable for the primary coating and may or may not be (in the case of a dual coating system) the same end as the primary coating , As long as there is no negative reaction to the chemistry of the terminal functional group (such as amine and system and cationic curing system). Compositions "hybrid" with this primary coating 49 200401912 Substances can also be used in this secondary coating. a. An oligomer A first component (I) of the secondary coating composition may be an aliphatic ethyl amino phosphonate oligomer based on a polyester and / or polyether and containing a reactive end .

The oligomers commonly used in UV curing systems include acrylated polyester, epoxy, and urethane. Acrylic polyesters are not good because they are easily hydrolyzed by high temperature hydrolytic aging. Regarding acrylic urethanes, aromatic and aliphatic isocyanate-based urethanes are suitable. Aliphatic urethanes do not have the disadvantages of poor thermal and oxidative stability. When using polyether-based urethanes, various thermal stabilizers and antioxidants may need to be added.

It is also possible to use urethanes based on polyester and / or polyether mixtures. This mixture can be formed by mixing a preformed end-reacted polyether urethane and a preformed end-reacted polyester urethane, or a mixed batch can be prepared by mixing the polyester units and polyether units with an isocyanate guide (precursor) to form a mixed oligomer, and then add the reaction end. However, it is the functional group backbond rather than the end group of the oligomer, which gives the composition good characteristics. Therefore, it is based on the above acrylate or fluorenyl acrylate 50 200401912

A similar system of the base composition (but possessing any reactive terminal functionalities) meets this requirement equally. Therefore, this methacrylate can be partially or completely replaced by terminal functional groups of various other examples (which can be reacted by irradiation or other methods (either induced by free radicals or cured by cations) to provide a coating that performs well . These terminal functional groups include free radical systems, such as thiolene systems (based on the reaction of polyfunctional thiols and unsaturated polyenes, unsaturated polyenes such as ethylene 6 | (vinyl ether); ethyl Dilute sulfide; allylic ether and bicyclicene); amine-ene system (based on polyfunctional amine and unsaturated polyvalent dilute reaction); acetylene System; the reactive part of the compound in the system is in the molecule rather than at the end; other ethylene (such as styrene) systems; acrylamide systems; allylic systems; itaconic acid Systems and crotonate systems; and cationic curing systems such as onium salt-induced vinyl ether systems and epoxy-terminated systems (which react by ring opening) ; And any other teachings taught to Shustack in U.S. Patent No. 5,639,846, which is incorporated herein by reference in its entirety, possesses a reactive end-based compound. It is foreseeable that virtually any terminal functional group does not adversely affect the desired properties of the cured composition (ie, oxidative, thermal, and hydrolytic stability and moisture resistance) when cured by irradiation or other methods. Compounds that can be used as terminal coating monomers include, but are not limited to, acrylic acid 51 200401912

Esters, methyl propionate, vinyl ether, vinyl su lfide, allylic ether, bicyclicene, mercaptan, acetylene ( acetylene), epoxide, amine, styrene, acrylamide and others. Suitable for use as a terminal-coated monomer. Hydroxyl-terminated compounds include, but are not limited to, hydroxyethyl acrylate; Hydroxypropyl acrylate; hydroxypropyl methacrylate; hydroxybutyl aery late; hydroxybutyl methacrylate methacrylate); allyl ether; hydroxyethyl vinyl ether; hydroxypropyl vinyl ether; hydroxybutyl vinyl ether; Hydroxyethyl mercaptan; hydroxypropyl mercaptan; hydroxyethyl-3-mercaptopropionate; and hydroxy-3 -Hydroxypropyl-3-mercaptopropionate. A suitable base bond polymer is then an aliphatic urethane polymer having a polymer and / or polyether backbone, such as an acrylate aliphatic urethane oligomer, Contains 70% oligomer solids in a hexanediol diacrylate solvent. A suitable broker is from j7〇rest park 52 200401912

Eastman Chemical has a component name of 015-1516, which contains 75% by weight of a polyester and / or polyether-based acrylate aliphatic urethane oligomer and hexanediol diacrylic acid. 25% by weight polyether in the ester solvent. Another suitable oligomer is PHOTOMER 6008, which is a polyether-based acrylate aliphatic urethane oligomer available from Cognis, Ambler, PA. In addition to the acrylate ends, other ends can also be used for this primary or secondary coating. Examples of other suitable oligomers include PHOTOMER 6008 (monthly aliphatic urethane acrylate), PHOTOMER 6019 (51% acrylate oligomer, tripropylene glycol diacrylate 48.08 %, Hydroquinone (0.9%, and acrylic acid 0.02%), all manufactured by Cognis; amidinopropionate oligomers purchased from UCB, Smyrna, Georgia; Sartomer, purchased from Exton, Pennsylvania E10010 (polyether urethane diacrylate); purchased from Eastman Chemical 015-1516 (urethane acrylate oligomer 75%, 1,6 hexanediol diacrylate) Acrylate 25%); CN 969 (S acrylic oligomer) from Sartomer; PHOTOMER 6010 (2-Hydroxyethylacrylate-4-4'methylenebis (cyclohexyl isocyanate)) from Cognis -Polytetramethylene glycol polymer (2-hydroxyethyl acrylate-4-4 'methylene bis (cyclohexylisocyanate) -polytetramethylene glycol polymer) 87%, trimethylene alcohol propylene glycol polyethylene glycol ether triacrylate 53 200401912 trimethylolpropane polyethylene glycol ether triacrylate) 13%) and mixtures thereof. The oligomer component includes the total weight of the secondary coating composition and the dry solid base from about 10% to about 90% by weight, and the percentage is based on the amount of the polymer alone. b. Viscosity-adjusting compounds that interfere with hydrogen

A second component of the secondary coating composition is a viscosity adjusting component (II) of a hydrocarbon compound which can react with the terminal of (I). One of the functions of this compound is to adjust the viscosity of the coating so that the coating can be easily applied to fibers having a buffer coating. The compound can be a hydrocarbon in nature to provide its hydrophobicity and make it compatible with other systems, and can include a bicyclic structure to minimize shrinkage during curing.

Such suitable compounds include, but are not limited to, isobornyl acrylate; isobomyl methacrylate; six to sixteen saturated hydrocarbon glycol acrylates or fluorenyl acrylates Esters, such as a mixture of C14 and C15 diol diacrylates or dimethacrylates of fourteen carbons and fifteen carbons, hexanedipropylene glycol Hexanediol diacrylate or hexanediol dimethacrylate; hexanediol dimethacrylate; isobomyl vinyl ether; six to sixteen carbon saturated hydrocarbon diols C6 to C16 saturated hydrocarbon diol vinyl ethers) such as hexanediol divinyl ether or cyclohexane dimethanol divinyl ether; six to sixteen carbon saturated diols Stone dangerous alcohol 54 200401912

(C6 to C16 saturated dithiols) such as hexanedithiol, decanedithiol, and CyCiohexane dimethanol dithiol; six to sixteen carbon saturated carbons C6 to Cl6 saturated hydrocarbon terminal dioxides such as tetradecane dioxane < tetradecadiene dioxide; six to sixteen carbon saturated hydrocarbon terminal diglycidol scales (C6 to Cl6 saturated hydrocarbon terminal diglycidyl ethers) such as hexanediol diglycidyl ether; or a mixture of these compounds (as long as these mixtures will be coreactive but not negative to the ingredients used in (I) reaction). A mixture of isobornyl acrylate and hexanediol diacrylate (the hexanediol diacrylate provides a reaction solvent as an oligomer) is a suitable ingredient .

The second component is generally a monomer or a mixture of monomers. Suitable monomers include SR238 (1,6 hexanediol dipropionate 99.09%, hydroquinone monomethyl ether 0.001 ° /.) Purchased from Sartomer; CD614 (polypropylene glycol Polypropylene glycol nonphenyl ether acrylate, 99.50%, poly [oxy (methyl-1,2-acetamidine)], α- (nonaphenyl) -ω-hydrogen- (poly [oxy (methyl- 1,2-ethanediyl)], a- (nonphenyl) -0-hydroxy-) O.5O〇 / 〇); IBOA (exo-propionate isobornyl vinegar) from UCB; SR 339 from Sartomer ( 2-phenoxy ethyl acrylate (99.91%, hydroquinone monomethyl ether 0.09%); HDODA (1,6 hexane di) from UCB Alcohol diacrylate); SR-339 (2-phenoxyethyl acrylate) 99.91%, p-phenylenediphenyl monomethyl ether 55 200401912 from Sartomer

(hydroquinone monomethyl etiier) 0 · 09%); from Sartomer's SR 349 (bispan A polyethylene glycol diether diacrylate) 99.91%, terephthalate Ether 0.09%); TMPTA (99.9% trimethylolpropane triacrylate, 0.1% terephthalate methyl ether); and ISC special purpose purchased from Tarrytown, New York ARONIX Ml 17 (99% for polypropylene glycol nonphenyl ether acrylate, 1% for toluene) from Chemical Company. Ingredient (II) comprises from about 20% to about 60% by weight of the composition based on the total weight of the dry solid basis of the (I), (II) and (III) ingredients. c. Photoinitiator

For example, in the primary coating ’a photoinitiator (III) is a possible component of the secondary coating but (without the use of a radiation system) is only required for curing in ultraviolet UV light. Any of the aforementioned photoinitiators tried for primary coatings can be used. Preferred photoinitiators are hydroxycyclohexylphenyl ketone and (4-octyloxyphenyl) phenyl iodonium hexafluoro antimonate. The photoinitiator can be added in an amount that can effectively induce curing of the composition and includes a weight percentage of from about 0.05% to about 100% based on the total weight of (I), (II), and (III). / 〇. Suitable photoinitiators include IRGACURE 184 (1-hydroxycyclohexylphenyl ketone) commercially available from Ciba Specialty Chemicals, Tarrytown, New York; Cyclohexylphenyl ketone) and mixtures thereof. In general, lower level photoinitiators are acceptable and although not necessary, they may be better used in this secondary coating than in primary coatings. d. Non-essential additives

Just as in the main coatings, a variety of available non-essential additives (IV) such as stabilizers include, but are not limited to, one or more organic phosphites, hindered phenols, hindered amines, Certain silanes and their mixtures and their analogs. A typical stabilizer is thiol diethylene di [3_ (3,5_di-third-butyl-4-hydrophenyl) propionic acid] CAS # 41484-35-9. When used, the amount of the stabilizer is from about 0.1% to about 3% by weight based on the total weight of the fluorene oligomer, (II) monomer, and (III) photoinitiator.

Suitable stabilizers include SILQUEST A-1110 ((γ-aminopropyl) trimethoxysilane 98%, methanol 2%) available from Crompton (OSI) of Palatine, Illinois; and IrgANOX 1035 (benzenepropanoic acid) from Ciba Specialty Chemicals ° Another non-essential additive for secondary coatings is a surface tension adjustment silicone resin additive, which can be used in secondary coatings Examples of application to a cured primary coating. Suitable surfactants include Tego 57 200401912 from Essen, Germany

Chemie's TEGO RAD 2200N (silicon polyether acrylate 98%, light aromatic solvent naphtha (petroleum) 2%); DC from Dow Corning, Midland, Michigan ADDITIVE 57 (siloxane and silicon, di-methyl, 3-hydroxypropyl methyl, polyethylene glycol acetate glycol acetate) 88%, polyethylene glycol monoallyl ether acetate 90 / 〇, poly (oxy-1,2- ethyl alcohol) (X- ethyl blue co- (ethynyloxy)-(poly (oxy-1,2-ethanediyl)

a-acetyl-o)-(acetyloxy)-) 3%); SILWET L-7602 (siloxane) and silicon, di-methyl, 3-hydroxide from Crompton (OSI) Propyl methyl (3-hydroxypropyl methyl), ether added polyethylene glycol monomethyl ether 80%, polyoxyethylene allyl methyl ether (polyoxyethylene allyl methyl ether) 20% ): BYK 371 (xylene) 48%, acrylic_functional dimethylpolysiloxane 40%, ethylbenzene 12%) from BYK Chemie, Wesel, Germany ; BYK 361 (acrylic co-polymer) 98%, light aromatic solvent naphtha (petroleum) 2%, purchased from BYK Chemie; modified BYK371 (acrylic functional group two) Acrylic-functional dimethylpolysiloxane 58 200401912 70%, 1,6 hexanediol diacrylate (30%, xylene 1%) and mixtures thereof. A crosslinking agent may optionally be included in the secondary coating.

A chain transfer agent may be included, such as IOMPA (isoctyl 3-mercaptopropionate) manufactured by Hampshire of Nashua, New Hampshire. Finally, the secondary coating may contain an adhesion promoter, such as SILANE A-172 (vinyltris (2-methoxyethoxy) silane) from Crompton (OSI) 95%, polysiloxane 3.5% (impure), 2-methoxyethanol (1.5%); Silane Α · 189 ((γ-Hydroxythiopropyl) from Crompton (OSI) Radical) trimethoxysilane

((y-mercaptopropyl) trimethoxysilane) 85%, (3-chloropropyl) trimethoxysilane 15 ° / 〇); and acrylated polysiloxane For example, acrylic polysiloxane from Tego Chemie, Essen, Germany, and mixtures thereof. A secondary coating composition suitable for applying to an optical fiber comprises: (I) a polyester and / or polyether based acrylate aliphatic amino group from about 40% to about 80% by weight Ethyl oxalate phytopolymers, and (II) weight percents of isobornyl acrylate 59 tablets from about 25% to about 50% and hexanediol diacrylate Mixture; and (III) hydroxycyclohexylphenyl ketone from about 2% to about 7% by weight, all of the above weight percentages are based on (I), (II), and (III) Based on total weight. The composition may also include a stabilizer, such as a mercaptan diethylene di (3,5-di-third-butyl-4-hydrogen), in an amount of from about 0.5% to about 1.5% by weight (based on the weight of the composition). Oxygen) thiodiethylene bis (3,5-di_tert-butyl-4-hydroxy) hydrocinnamate. As a result, in a specific embodiment, a description of the type and amount of the bridging agent used for the main coating may also be used here. In the embodiment, the surface tension adjusting additive may also be included therein and the oligomer component (I) may be a mixture of aliphatic urethane acrylate oligomers having polyether as a backbone. Since the conventional method for filtering the secondary coating before coating on the glass fiber cannot avoid the generation of spot-like bumps, the focus of the present invention is particularly on changing the filtering conditions. The following is a typical secondary coating, as described in U.S. Patent No. 6,048,911 to Shustack et al., Which is incorporated herein by reference in its entirety. Mono aliphatic urethane acrylate; hexanediol acrylate (HDODA); a photoinitiator containing IRGACURE 184 (1-hydroxycyclohexylbenzene 200401912 based ketone) and a primary antibody The oxidant contains IRGANOX 1035 (—hindered polyphenol); a silicon acrylate compatibility agent such as BYK-371; a functionalized silicone compound such as TEGO Rad-2100, TEGO Rad-2200; and

Non-essential conventional additives such as heat stabilizers and the like include, for example, organic phosphates, hindered phenols, hindered amines, and mixtures thereof. Other suitable secondary coating compositions include KLEARSHIELD 1-001, KLEARSHIELD 2-002, KLEARSHIELD 1-002, KLEARSHIELD 2-001, BONDSHEILD 5-001, BONDSHIELD 5-002 commercially available from Boden Chemical Company, Columbus, Ohio. , KLEARSHIELD 4-001, and DATASHIELD 6-002.

Table 1 shows the individual components of a typical secondary coating (Paint A) and is expressed in weight percent: 61 200401912 Table 1 Ingredient%, Weight Percent Propionate Monomer 1 15.66 Acrylic Monomer 2 Starter 3.98 Inhibitor 0.99 Acrylic monomer 13.89 Acrylic oligomer 32.73 Methacrylic oligomer 32.73 Surfactant 0.02

Coating A can be formulated in a series of steps in the following manner. First, the light initiator, functionalized silicone 'antioxidants, other additives, and half of the acrylic single system were mixed in a clean, well-ventilated tube for 1.5 hours. This mixture is kept in reserve and is provided after continuous mixing. In the next step, 70% of all acrylic oligomers are heated to 140QF to help them be drawn into a kettle. The oligomer was agitated slowly and kept at a temperature below or equal to 105 ° F. The mixture obtained in this first step is sucked into the oligomer in the pot. The remaining oligomers were then added to the pot. The mixture obtained when 30% of the acrylic monomer was added was stirred and mixed at a higher rate 62 200401912 for 30 minutes. Examples

The following viscosities in Table 2 are based on a Brookfield viscometer (with a constant temperature bath and a sample cup, using the number SC4-34 spindle (spindle), speed 6 rpm) for the coating composition of coating A (as described above) at various temperatures Measured. The filter used is a Calyx Cartridge, WN grade, a silicon filter, code 5. It has a hole size of 0.45 μ, such as Catalog No. WN04000A51'Material No. 1212686, which is available from Osmonics Corporation of Minnetonka, Minnesota. Table 2 Temperature (° c) Measured viscosity (mPa) 25 4879 30 3159 35 2110 40 1440 45 1030 50 725 55 550 60 415

The above information is shown graphically in Figure 11 and illustrates the direct dependence of the viscosity on temperature. The linear regression analysis of the data in Table 2 is shown in the following formula II: (Π) Ι ^) = 6992.5 (1 / Γ) -15.025 63 200401912 where η is the viscosity in mPa · s as the measurement unit and T is regarded as the absolute temperature (Kelvin (° C +273)) is the temperature in units of measurement. In addition, it should be noted that R2 produced by linear regression is 0.998. Therefore, the formula III can be used to calculate the viscosity at any temperature: 7? = Β (69922 / Γ) -15.025 ⑽

Where η is the viscosity with mPa.s as the measurement unit and T is regarded as the temperature with the absolute temperature as the measurement unit. Although the results of these observations and calculations were determined by Coating A as described above, the same viscosity measurements and calculations can be repeated on the actual coating composition. When the coating composition is changed, the specific numbers shown in Equations II and III will change, but the general relationship between the natural logarithm of the year and the temperature remains unchanged. When the filter coefficient (γ) is as described in the following formula I: AP (mPa)

(1) r] (mPa.s) -Y (S where η is the viscosity and the filter coefficient (γ) is kept below or equal to 250,000 s · 1, the maximum temperature and pressure difference can be determined. Table Three provides the two temperatures under several pressure differences when the filter coefficient is 250,000 s · 1. Table 3 Pressure difference (psi) Maximum temperature (° C) 0.5 123.2 5 77.5 64 200401912 10 65.7 20 54.7 30 48.6 40 44.4 50 41.2 60 38.7 70 36.5 80 34.7 90 33.1 100 31.7

This information is shown graphically in Figure 12. Table 4 provides the maximum pressure difference at several sample filtration temperatures, where the filter coefficient is limited to a maximum of 250,000 s_1. Table 4 Temperature (° c) Maximum pressure difference (psi) 0 1438.7 5 907.6 10 582.0 20 250.4 30 113.9 40 54.5 50 27.3 60 14.2 70 7.7 80 4.3 90 2.5 100 1.5

This information is shown graphically in Figure 13. The above calculation is based on a maximum filter factor of 250,000 s · 1, where ΔP / η = 250,000 s · 1. From the data in Table 3 and formulas I, II, and III, the graphs of Figure 12 to 65 200401912 and Figure 13 are generated. The graph shown in Fig. 12 illustrates the maximum pressure difference at which the filtration factor of 250,000 is reached at the given filtration and temperature. In particular, the graph illustrates that at a given temperature, any pressure difference below the curve will cause the filter coefficient to be less than or equal to 250,000 s-1. This curve represents a parameter that achieves a filter coefficient of 250,00 s_i, so that any pressure difference below this curve will necessarily provide a suitable over-coefficient. In addition, this curve illustrates that as the filtration temperature increases, the respective maximum pressure differences decrease. Although not wishing to be bound by any theory, it is believed that at higher temperatures, the gel-like composition becomes more elastic and soft, so the force caused by pressing the gel against the filter will more easily tear The gels (or make them softer to squeeze through the filter holes) and allow continuous flow through the perforations. Similarly, as the temperature decreases, the maximum pressure difference increases. As such, it is believed that the gel has the asexuality and softness of Car J at lower temperatures, resulting in this result. Therefore, a larger force is required at a lower temperature to tear or squeeze the gel composition. The graph shown in Fig. 13 details how the maximum filtration temperature is affected when the overpressure rises, so that the filtration coefficient is at the upper limit of 250,000. Figure 13 illustrates that as the pressure difference increases, the maximum temperature decreases. As described in relation to Figure 12, it is believed that because the higher pressure difference causes greater pressure on the gel, lower temperatures are needed to avoid the force tearing the gel and forcing the gel through the filter, pores. As long as the selection temperature is below the curve, the obtained filter coefficient will be maintained at a level of less than or equal to 250,000 000 200401912. It should be noted that the change in pressure listed on the X axis is the overall perceived pressure across the filter. Therefore, this graph takes into account the number of filters, whether parallel or continuous, and their surface area. If this factor is changed, changing the overall perceived pressure will result in different maximum temperatures. Following the process outlined above, the same calculations can be applied to any coating composition. The main process is as follows:

1. Measure viscosity (η) at various temperatures (T) to determine its mathematical relationship to complete the general formula IV (IV) \ η (η) = α (γ) -l · b where η is the viscosity , Tested in units of mPa.s, and T is the temperature tested in absolute temperature. 2. Once the values of a and b are calculated through a linear regression analysis obtained from the data in the first step, it can be determined that the relationship between the viscosity and the pressure difference makes any filter coefficient limited to a maximum of 250,000 S_1. Specifically, formula III can be used to calculate filter coefficients for various viscosities (determined by filtration temperature) and pressure differences. 3. Then select a suitable viscosity and pressure difference to keep the maximum value of the filtration coefficient at 250,000 s · 1, and also limit a variety of other filtering, costs' for example to generate heating temperature and pressure difference and the energy of the total filtration flow . According to the above-mentioned general calculation formulas for passing pressure differences, viscosities of various filter media, and temperature of 200420041212, the present invention obtains a formula that can be used to maintain filtration to remove spot-like bumps. Specifically, the following formula v can be used to determine the maximum pressure difference (△ P) across each filter medium at a given temperature:

AP max (/ 75 /) _ ^ max (l / s) X TJ (mPa s) 6.894757 (mPa / psi) (V)

Wherein η is the viscosity of the coating composition at the specific temperature, and γ is the maximum preferred filter coefficient. Therefore, when the filter coefficient is maintained below 250,000 s · 1 or below 250,000 s · 1, the pressure difference is calculated according to the following formula: AP 250000 (\ / S) X 6 6992 5 (mPa s K), Γ (〇 + 273, -15 025 (mPas) (VI) m3X (psi) —— 6.894757 (mPa / psi) where T is the filtration temperature (in Celsius) of the individual filter media. By using formulas V and VI, the following formula The VII series is determined to maintain the maximum value of the filter coefficient at the maximum value of filtration and temperature:

T max (C) ——

In 6992.5c mPa s K) -273 (_) χ 6.894757 (^, max (i / s) psi) —15.025 (^ where T is 68 under a pressure difference ΔP of the maximum filter coefficient γ (VII) 200401912 to the maximum filter temperature. However, the above formula ι-νπ can be used to select any filter coefficient less than or equal to 250,000 s · 1. The invention has decided that the filter coefficient of the coating composition that will pass through at least one filter medium Limiting it to less than about 250,000 s-1 reduces or eliminates the number of spotted bumps. There are several examples of filtering processes that illustrate the benefits of keeping the filter coefficient below about 250,000 s-1.

The coating composition typically used in the filtration method of the present invention is filtered under various temperatures and pressures. The detailed results are shown in Table 5. In the example shown in Table 5, the filter used is a 10-inch nylon, Calyx Cartridge, WN grade, silicon filter (code 5) with a hole size of 0.45 μ, such as Catalog No. WN04000A51, Material No. 1212686, which are available from Osmonics Corporation of Minnetonka, Minnesota. Table 5 Coating temperature (° F) Pressure difference (psig) Filter coefficient (sj result B-1 105 60 284,802 Failure B-2 105 40 189,868 Success B-3 90 40 103,306 Success B-4 105 15 71,200 Success B-5 70 40 43,479 Success 69 C-1 105 60 284,802 Failure C-2 90 60 154J26 Success C-3 90 40 103,306 Success 200401912 In Table 5, the pressure difference and filter coefficient are used in the overall filtration system. For B-1, the The pressure difference of 60 psi is the overall pressure difference of the filter system having a plurality of filters arranged in parallel in two consecutively arranged casings. Therefore, the pressure difference in Table 5 is from the entrance of the first casing to the first The outlet of the second case. However, the first case has a pressure difference of 5 psi, and the pressure difference between the two cases is negligible. The pressure difference of B-2, B-3, and B-5 is 40 psi. It is the overall pressure difference of a filter system with a filter housing containing a plurality of filters arranged in parallel. Therefore, the pressure difference in Table 5 is from the inlet of the filter housing to the outlet of the filter and housing. For B_4, the pressure The difference is that having multiple The overall pressure difference of the filter system of the filters arranged in parallel in the consecutively arranged shells. Therefore, the pressure difference in Table 5 is from the inlet of the first shell to the outlet of the second shell, but the pressure of the first shell The difference is 0, and the pressure difference between the two shells is negligible. For C-1 and C-2, the pressure difference of 60 psi is for the case where there are multiple parallel in two consecutively arranged shells. The overall pressure difference of the filter system of the arrayed filters. Therefore, the pressure difference is from the inlet 70 200401912 of the first housing to the outlet of the second housing. However, the first housing has a pressure difference of 5 psi and the first The second case has a pressure difference of 55 psi, and the pressure difference between the two cases is negligible. The C-3 pressure difference of 40 psi is a filter with a filter case containing a plurality of filters arranged in parallel. The overall system pressure difference. Therefore, the pressure difference in Table 5 is from the inlet of the filter housing to the outlet of the filter housing π 〇

In the example in Table 5, the results are determined by the proportion of point bumps. As mentioned above, in some cases, an average of 5-10 point bumps per kilometer is tolerable, expressed as "success", although in other cases an average of 0-5 point bumps per kilometer is required, And although in other cases it is required to completely remove the stippled bumps, that is, there are 0 stippled bumps in the entire filtration product. In addition, other examples have shown that coating materials obtained with filter coefficients between about 50,000 and 190,000 s_1 produce optical fibers with a frequency that reduces or removes the appearance of point bumps in typical factory products.

Coating B consists of KLEARSHIELD 2-002 (purchased from Boden Chemical Co., Columbus, Ohio). Coating C consists of KLEARSHIELD 2-001 (purchased from Boden Chemical Columbus, Ohio). Coating B and Coating C are manufactured according to the process described in US Patent No. 5,527,835 issued to Shustack. Although the present invention has been described with reference to preferred embodiments, it should be readily understood that many variations and / or modifications can be made to the invention without departing from the spirit of the invention. For example, it should be noted that the filtration process of the present invention can be used for coating products at any stage, coating and curing from raw manufacturing materials to a drawing table. Therefore, it is considered to fall within the scope of the invention to filter the ingredients before mixing to become a secondary coating and to filter all ingredients simultaneously after mixing and before use in a stretching table.

In addition, any coating composition can be filtered by the filtration technique of the present invention. Although the present invention has been disclosed for use in filtering coatings for optical fibers, it is considered to fall within the scope of the present invention to filter any coating composition provided on the surface of any point where it is desired to remove point bumps. Therefore, the aforementioned filtering process can be used to manufacture other items such as optical media, such as compact magnetic disks and digital video and magnetic disks, dental compositions (such as teeth), and laminated surfaces. In any case, the invention is limited only by the scope of the following patent applications. [Schematic description]

FIG. 1 is a view along a longitudinal axis of a coated optical fiber, wherein the coated fiber has no dot-like bumps; FIG. 2 is a view along a longitudinal axis of a coated optical fiber, where the The coated optical fiber has external dot-like projections; FIG. 3 is a view along the longitudinal axis of a coated optical fiber, wherein the coated optical fiber has internal dot-shaped projections; A view of the longitudinal axis of a coated optical fiber, wherein the coated optical fiber has a punctiform bump having internal and external features; 72 200401912. Fig. 5 is a diagram showing the optical fiber coating process according to the present invention, and Fig. 6 is a diagram showing the filtration process of an optical fiber coating according to the present invention; Fig. 7 is based on A partial plan view of a membrane filter used in the present invention; FIG. 8 is a cross-sectional view of a central filter used according to the present invention; and FIG. 9 is an overall perspective view of a device for stretching glass fibers Figure 10 is a partial cross-sectional view of a device for applying a coating composition; Figure 11 is a chart illustrating the correspondence of viscosity to temperature; Figure 12 is a chart illustrating a method according to the present invention The maximum temperature used under different pressure differences; and FIG. 13 is a graph illustrating the change in the maximum pressure according to the temperature used according to the present invention. Description of the drawing number · 110 optical fiber 112 glass fiber 114 primary coating 116 secondary coating 120 optical fiber 122 glass fiber 124 primary coating 126 secondary coating 128 dot bumps 200401912 130 optical fiber 132 glass fiber 134 primary coating 136 times Primary coatings 138 Point-shaped bumps 140 Optical fibers 142 Glass fibers 144 Primary coatings 146 Secondary coatings 148 Point-shaped bumps 160 Provide primary coatings 161 Provide secondary coatings 162 Provide preforms 164 Stretch fibers 166 Apply primary coatings 168 Applying the secondary coating 170 UV curing 172 Winding 182 Mixing the secondary coating ingredients 183 Cooling 184 Filtration 201 Protector 202 Sheet 203 Filter film 204 Sheet 205 Core 206 End plate 207 Seal 208 Exit 310 Filter Medium 311 Fold 312 Support core 311 Support cage 20 Device 21 Optical fiber 22 Preform 23 Heating furnace 24 Device 25 Device 26 Center gauge 27 Ultraviolet light device

74 200401912 29 Winch 57 Shaft 62 Coating coater 64 Cushion pad 65 Housing 66 ° Spiral octagonal inlet 67 Cylindrical channel 68 First slot cavity 69 Lower portion 70 Cylindrical channel 71 Second slot cavity 72 Compared Lower part 73 cylindrical passage 76 line 77 line 81 die 82 die 84 die opening 86 die opening 88 die opening 93 flow channel 94 first coating material

75

Claims (1)

200401912 Patent application scope: 1. A method for forming a coating on a substrate, comprising: providing a coating composition; passing the coating composition through at least one filter including at least one filter A filtering device of the filtering assembly filters the coating composition, and applies the filtering and subsequent coating composition to the substrate; wherein the at least one filtering assembly has a filtering coefficient determined by a formula I (γ) (I) fiber, -1) The filter coefficient (γ) is a maximum of 2500003 ^, which is the viscosity of the coating composition with the individual temperature in the individual filter assembly, and ΔP is the span across the individual The pressure difference between at least one filter and the assembly, the pressure difference is between about 0 to about 80 psig, and the pore size of the at least one filter and the filter of the at least one filter assembly is a maximum of 10 μm, and The individual temperature of the coating composition in the at least one filter assembly is a maximum of about 120 ° F. 2. The method for forming a coating on a substrate as described in item 1 of the scope of the patent application, wherein the maximum pressure difference during the filtration process is determined by AP max (psi) ^ max (l / s) XT ^ j (mPa s) 6.894757 (w / w _) and the first draft of the USERVERA program \ 00703-TW-patent specification doc 76 200401912 AP 250000ο / S) Xe 6992.5 (mPa s K) ~~ Γ (〇 + 273 — 15.025 (w ^ a (max) (psi) — 6.894757 (^ / psi) is selected by the selected group *, where 7? Is the viscosity of the coating composition in the individual filter assembly at the operating temperature T, and γ is the maximum preset filter coefficient. 3. The method for forming a coating on a substrate as described in item 1 of the scope of patent application, wherein the maximum temperature during the filtration process is determined according to the following formula: max (C) In _6992.5 (, ΔP (㈣ x 6.894757 (mPa / psi) -273 ϊ max (i / -15.025 (, where ΔP is the pressure difference across each individual filter assembly, and 7? It is the viscosity of the coating composition in the individual filter assembly at the filtration temperature T, and the preset filter coefficient for the maximum γ system. 4. The method for forming a coating on a substrate as described in item 1 of the scope of patent application, wherein at least one of the filters of the at least one filter assembly has a filter coefficient of up to 250000s, and its pores The size is in the range of about 0.05 μm to about 5 μm, and wherein the filtration is performed at a temperature of less than about 105 ° F (40 ° C) and a pressure difference across the individual filtration assemblies is at a maximum of about 80 psig. 5. Such as The method for forming a coating on a substrate as described in item 1 of the scope of patent application, wherein the substrate is an optical fiber. 6. The method as described in item 5 of the scope of patent application for use on a substrate A method of forming a coating layer \\ SERVER \ program draft \ 00703-TW · patent specification doc 77 200401912 layer, wherein the coating composition is coated on the optical fiber as a secondary coating; and further includes the following steps: the optical fiber Applying a primary coating composition, wherein the secondary coating is applied on the primary coating. 7. The method for forming a coating on a substrate as described in item 6 of the scope of patent application, Also includes: curing the main Coating; and thereafter curing the secondary coating on the optical fiber. 8. The method for forming a coating on a substrate as described in item 6 of the patent application scope, wherein the primary coating is cured simultaneously And curing the secondary coating. 9. The method for forming a coating on a substrate as described in item 1 of the scope of the patent application, wherein the filtering is performed at a temperature of about 60 ° F to about 95 ° F. 10. The method for forming a coating on a substrate as described in item i of the scope of patent application, wherein the filtering is performed at a temperature of about 70 ° to about 90T. 11. The method for forming a coating layer on a substrate as described in item 1 of the scope of patent application, wherein the filtering is performed at a temperature of about 70 ° to about 80 °. 12. The method for forming a coating on a substrate as described in item 丨 of the scope of patent application, wherein the at least one filter assembly has a filter coefficient of less than or equal to about 43000s ". 13. As a patent application The method for forming a coating on a substrate as described in the range item 丨, wherein the at least one filter assembly has a filter coefficient in a range of about 50,000 s · 1 to about 19,000 si. The method for forming a coating on a substrate as described in the scope of the patent application, wherein the pressure difference of the filtration is about 35 to about 55 psig \\ serverA program draft \ 00703-TW-patent specification d〇 c y 200401912 15 > 16, 17, 18 19 20 21 22, WSERVERA program beginning 79 The method for forming a coating on a substrate as described in the first patent application scope, wherein the pressure difference of the filtration is About 40 to about 50 psig. The method for forming a coating on a substrate as described in item 1 of the patent application scope, wherein the at least one filter assembly includes a membrane filter, the membrane filter The device has a range from about 0.05 to about 0.0 6μηι pore size. • The method for forming a coating on a substrate as described in item 1 of the scope of patent application, wherein the at least one filter assembly includes a membrane filter, and the membrane filter has A hole size of about 0.1 to about 45 μm. The method for forming a coating on a substrate as described in item 1 of the patent application scope, wherein the at least one filter and assembly includes a central filter ( depth filter), the central filter has a pore size from about 0.5 to about 5 μm. k The method for forming a coating on a substrate as described in claim 1 of the patent application scope 'wherein the at least one filter The assembly includes a central filter having a pore size from about 1 to about 3 μm. 'Method for forming a coating on a substrate as described in item 1 of the scope of patent application', wherein the The substrate is a cornpact disk or a digital video disk (DVD). 'The method for forming a coating on a substrate as described in item 1 of the patent application scope, wherein The substrate is ≫ The method for forming a coating on a substrate as described in item 1 of the scope of patent application, wherein the coating composition is a dental composition 〇 draft \ 〇07〇 3-Ding-Patent Specification doc 200401912 23 24 25, 26, 27, 28, 29 30 31 \\ SERVER \ Procedure A method for forming a coating on a substrate as described in item i of Shengu Patent Scope 'Wherein the substrate is a laminated surface. ‘The method for forming a coating layer on a substrate as described in item 丨 of the patent application scope, wherein the filter device includes a plurality of transition assemblies arranged continuously. The method for forming a coating on a substrate as described in the scope of the patent application, wherein the filtering device comprises a plurality of filtering assemblies arranged in parallel. The method for forming a coating on a substrate as described in item 1 of the scope of the patent application, wherein each filter assembly has a filter and a coefficient of at most 250,000 s-1. A product made by the method described in item 1 of the scope of the patent application, wherein the coated substrate is an optical fiber and the product has less than about 10 dot-like bumps per kilometer. A product made by the method described in item 1 of the scope of patent application, wherein the coated substrate is an optical fiber and the product has less than about 5 dot-like bumps per kilometer. 'A product made by the method described in item 1 of the scope of the patent application, wherein the coated substrate is an optical fiber and the product has 0 point bumps per kilometer. 'The method for forming a coating on a substrate as described in item 1 of the scope of the patent application, wherein at least one of the filters of the at least one filter assembly has a thickness of about 0.05 μm to about 5 μm The size of the pores in the range, and the filtration is performed at a temperature of less than about 10 μF (4 (rc)) and the maximum difference in M force across the to y transition assembly is about 80 psig. The method for forming a coating paper on a substrate according to the item described above, wherein the pressure difference is in the range of about 3 to about 40 psi. 32, such as applying for a patent The method for forming a coating on a substrate as described in the scope item 1, wherein the filter has a hole size in the range of about 0.45 to about 3 μm. 33. Use as described in the scope of the patent application scope item 1 A method for forming a coating on a substrate, wherein the filtration temperature is in a range of about 70 to about 105 ° F. 34. A method for filtering a coating composition, comprising: at a temperature and Under a pressure difference (ΔP), The filtering device of the assembly filters a coating composition having a viscosity so that the filtration coefficient of the at least one filter of the at least one filtering assembly obtained is not greater than 250,000 s · 1, wherein the pressure difference is Measured by the filter assembly, where ΔP is between about 0 to about 80 psig and the pore size of at least one filter of the at least one filter assembly is at most 10 μm, at a temperature of at most 120 ° F. 35. The method for filtering a coating composition as described in item 34 of the scope of patent application, wherein the maximum pressure difference during the filtering process is based on AP max (l / s) XT ^ j (mPa s) 6.894757 ( wiw_) and Δ max (/ 75 /) 250000 (\ / s) X 6 6992.5 (mPa s K), r (〇 + 273 —l5.025 (mPa i 6.894757 (mFa / \\ SERVER \ Preliminary Program \ 00703- TW-Patent Specification doc 81 200401912 selected from the group consisting of 7 / is the viscosity of the coating composition in the individual filter assembly at the operating temperature T, and γ is the maximum preset filter coefficient. 36. Used for filtering and coating as described in item 34 of the scope of patent application The composition method, in which the maximum temperature during the filtration process is determined by τ max (c) according to the following formula: 6992.5 (, K) In ΔΡ ^ οχ 6.894757, (mPa I-273 r max (i / 15.025 (, where ΔP is the pressure difference across each individual filtration assembly, and is the viscosity of the coating composition in the individual filtration assembly at the filtration temperature T 'and γ is the preset filter coefficient that is the largest. 37. The method for filtering a coating composition as described in item 34 of the scope of the patent application, wherein the filtering is performed at a pressure difference of a maximum of about 80 psig and a temperature in a range of about 50 to about 140T. 38. The method for filtering a coating composition as described in item 34 of the scope of the patent application, wherein the at least one filter assembly includes a membrane filter having a thickness of from about 0.1 to about 3 μm. Hole size. 39. The method for filtering a coating composition as described in item 34 of the scope of patent application, wherein the filtering is performed at a temperature in a range of about 60 to about 95T. 40. The method for filtering a coating composition as described in item 34 of the scope of the patent application, wherein the filtering is performed at a temperature in a range of about 70 to about 90T. 41. The method for filtering a coating composition WSERVERA preliminary draft as described in item 34 of the scope of patent application \ 00703-TW · patent specification doc g2 200401912, wherein the filtering is at about 70 to about 80 ° F Performed at temperatures in the range. 42. The method for filtering a coating composition as described in item 34 of the scope of the patent application, wherein the ratio of the pressure difference to the viscosity reduces the preset filter coefficient of the at least one filter assembly to less than or equal to 4300s_i 0 43. The method for filtering a coating composition as described in item 34 of the scope of patent application, wherein the filtration pressure difference in the at least one filtration assembly is about 35 to about 55 psig . 44. The method for filtering a coating composition as described in item 34 of the scope of the patent application, wherein the pressure difference of the filtration in the at least one filtration assembly is about 40 to about 50 psig. 45. The method for filtering a coating composition as described in item 34 of the scope of patent application, wherein the at least one filter assembly includes a membrane filter having a thickness of from about 0.05 to about 0.6 μm Hole size. 46. The method for filtering a coating composition as described in item 34 of the scope of patent application, wherein the at least one filter assembly includes a membrane filter having a thickness of from about 0.1 to about 0.45 μm Hole size. 47. The method for filtering a coating composition as described in item 34 of the scope of the patent application, wherein the at least one filter assembly includes a depth filter having a range from about 1 to about 4μιη hole size. 48. The method for filtering a coating composition according to item 34 of the scope of patent application, wherein the at least one filter assembly includes a central filter having a hole size from about 1 to about 3 μm . 49. A method for filtering according to item 34 of the scope of patent application, in which the pore size of the at least one transition assembly is about 0.05 μm to about 5 μm. -TW-Patent Specification doc 83 200401912 50 51 52 53 54 55 56 57 58 ^ \\ SERVER \ Initial program range, and the filter is at a temperature of less than about 105 ° F (400 ° C and the at least one filter) The pressure difference of the assembly is performed at a maximum of about 80 psig. The method for filtering a coating composition according to item 34 of the patent application scope, wherein the pressure difference is in the range of about 3 to about 40 psi. The method for filtering a coating composition described in the scope of patent application item 34 ', wherein the hole size of the filter is in the range of about 045 to about 3 μm. A method of filtering a coating composition ', wherein the filtering temperature is in a range of about 70 to about 105 ° F. The method for forming a coating on a substrate as described in item 49 of the patent application scope Method, wherein the substrate is an optical fiber. The method for forming a coating on a substrate as described in item 49, wherein the substrate is an optical medium. The method for forming a coating on a substrate as described in item 49 of the patent application scope. A method for forming a layer, wherein the coating composition is a dental composition. The method for forming a coating on a substrate as described in item 49 of the application, wherein the substrate is a laminate Surface A method for preparing a coated optical fiber, comprising: providing at least 50 tons of a coating composition in 12 months; filtering the coating composition; and coating an individual optical fiber with the coating composition In order to form a coated optical fiber that is several kilometers long, at least 98% of the coated optical fiber has less than about w dot-shaped bumps per kilometer. It is used to prepare a coated optical fiber as described in item 57 of the scope of patent application. The method of providing a coating composition includes providing a coating composition of at least -500 tons. 59. Use as described in item 57 of the scope of patent application To prepare A method for coating an optical fiber, wherein the step of providing a coating composition includes providing at least 1,000 tons of a coating composition. 60. The method for preparing a coated optical fiber as described in claim 57 of the patent application scope, wherein Or equal to 98% of the coated optical fiber has less than about 5 dot-shaped bumps per kilometer. 61. The method for preparing a coated optical fiber as described in item 57 of the patent application scope, wherein It is equal to 98% of coated optical fibers with less than about 2 dot-like bumps per kilometer. 62. The method for preparing a coated optical fiber as described in item 57 of the scope of the patent application, wherein greater than or equal to 98% of the coated optical fiber has less than about 0 point bumps per kilometer. 63. The method for preparing a coated optical fiber as described in item 57 of the scope of the patent application, wherein greater than or equal to 99% of the coated optical fiber has less than about 10 point bumps per kilometer. 64. The method for preparing a coated optical fiber as described in item 57 of the scope of the patent application, wherein greater than or equal to 99.75% of the coated optical fiber has less than about 10 spot-shaped bumps per kilometer 0 65. The method for preparing a coated optical fiber as described in item 57 of the scope of the patent application, wherein greater than or equal to 100% of the coated optical fiber has less than about 10 spot-shaped bumps per kilometer. 66. A product comprising the coating composition described in item 57 of the patent application scope of at least 50 metric tons. First, schema: \\ SERVER \ Draft of the program \ 00703-TW-Patent Specification doc 85