Low distortion interlayer
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26 claims: 4 independent, 22 dependent
- 1Patent claims Zastrzeżenia patentowe 1. Polymer sheet containing:poly (vinyl butyral);and a plasticizer, characterized in that said polymer has a surface with a waviness index less than 20,000 square micrometres and an R valuefrom at least 20 microns and durability between 10 and 95. 1. Arkusz polimerowy zawierający: poli(winylobutyral);oraz plastyfikator, znamienny tym, że wspomniany polimer ma powierzchnię o współczynniku falistości mniejszym niż 20.000 mikrometrów kwadratowych i wartości Rz co najmniej 20 mikrometrów oraz trwałość między 10 i 95.
- 6A method of producing a multilayer intermediate layer comprising the following steps:6. Sposób wytwarzania wielowarstwowej warstwy pośredniej obejmujący następujące etapy: forming a first polymer sheet containing poly (vinyl butyral) and a plasticizer, characterized in that said first polymer sheet has a first surface and a second surface and said first surface has a waviness index less than 20,000 square micrometres, R valuefrom at least 20 microns and durability between 10 and 95;formowanie pierwszego arkusza polimerowego zawierającego poli(winylobutyral) i plastyfikator, znamienny tym, że wspomniany pierwszy arkusz polimerowy ma pierwszą powierzchnię i drugą powierzchnię oraz wspomniana pierwsza powierzchnia ma współczynnik falistości mniejszy niż 20.000 mikrometrów kwadratowych, wartość Rz co najmniej 20 mikrometrów oraz trwałość między 10 i 95;placing the polymer film layer in contact with said first surface of said first polymer sheet to form a stack and laminating said stack. umieszczenie warstwy filmu polimerowego w zetknięciu ze wspomnianą pierwszą powierzchnią wspomnianego pierwszego arkusza polimerowego w celu sformowania stosu i laminowanie wspomnianego stosu.
- 18A method for producing a polymer sheet comprising forming a layer comprising poly (vinyl butyral) and a plasticizer, said layer having a first surface and a second surface and a waviness index less than 20,000 square micrometres, value 18. Sposób wytwarzania arkusza polimerowego obejmujący formowanie warstwy zawierającej poli(winylobutyral) i plastyfikator, przy czym wspomniana warstwa ma pierwszą powierzchnię i drugą powierzchnię oraz współczynnik falistości mniejszy niż 20.000 mikrometrów kwadratowych, wartość Rfrom less than 20 micrometres on said first surface, and embossing on said first surface a roughness template to produce said polymer sheet, characterized in that said polymer sheet has a waviness factor less than 20,000 square micrometres, R valuefrom at least 20 microns and durability between 10 and 95 on the side corresponding to said first surface of said layer. Rz mniejszą niż 20 mikrometrów na wspomnianej pierwszej powierzchni, i wytłoczenie na wspomnianej pierwszej powierzchni szablonu szorstkości w celu wytworzenia wspomnianego arkusza polimerowego, znamienny tym, że wspomniany arkusz polimerowy ma współczynnik falistości mniejszy niż 20.000mikrometrów kwadratowych, wartość Rz co najmniej 20 mikrometrów i trwałość między10 i 95 po stronie odpowiadającej wspomnianej pierwszej powierzchni wspomnianej warstwy.
- 26A method of making a multi-layer panel comprising the following steps:26. Sposób wytwarzaniapanelu wielowarstwowego, obejmujący następujące etapy: forming a first polymer sheet containing poly (vinyl butyral) and a plasticizer, where said first polymer sheet has a first surface and a second surface, and said first surface has a waviness factor less than 20,000 square micrometres, R valuefrom less than 20 microns and durability between 10 and 95;formowanie pierwszego arkusza polimerowego zawierającego poli(winylobutyral) i plastyfikator, gdziewspomnianypierwszyarkusz polimerowy ma pierwszą powierzchnię i drugą powierzchnię, zaś wspomniana pierwsza powierzchnia ma współczynnik falistości mniejszy niż 20.000 mikrometrów kwadratowych, wartość Rz mniejszą niż 20 mikrometrów i trwałość między10 i 95;contacting the polymer film layer with said first surface of said first polymer sheet to form a stack;zetknięcie warstwy filmu polimerowego ze wspomnianą pierwszą powierzchnią wspomnianego 15 pierwszego arkusza polimerowego w celu sformowania stosu;folding a glass layer with a polymer sheet of said polymer film;and laminating said stack. złożenie warstwy szkła z arkuszem polimerowym wspomnianego filmu polimerowego;oraz laminowanie wspomnianego stosu.
Independent claims4
286 paragraphs in 7 sections, as filed
The present invention relates to the field of multilayer glass panels containing a polymer sheet having desired surface properties, and more particularly the present invention relates to the field of multilayer glass panels comprising poly (vinyl butyral) having a finished surface with relatively low waviness and high roughness, in contact with poly (terephthalate ethylene) and / or other poly (vinyl butyral) layers.
BACKGROUND OF THE INVENTION [0002] Angstrom thick or thicker layers of metals, metal compounds and other substances are commonly used in multilayer glass panels to reflect solar infrared heat-producing radiation while transmitting visible light. These layers may be stacked in sequence and may be arranged on a suitable substrate, such as a biaxially stretched thermoplastic film of polyethylene terephthalate (PET) or similar material. One form, known as an interference filter, consists of at least one reflective metal layer sandwiched between reflection damping or anti-reflection dielectric layers.
[0003] When a metallized film, such as an interference filter, is combined with glass in a multilayer glass laminate, for example in the windshield of a vehicle, an impact-dispersing intermediate layer of softened poly (vinyl butyral) (PVB) is usually introduced to absorb head impact persons in a vehicle or foreign object from outside the vehicle, preventing penetration through the windscreen. In a typical configuration, a single layer of poly (ethylene terephthalate) film is sandwiched between two layers of poly (vinyl butyral) material, forming a three-layer structure, which in turn is sandwiched between two layers of glass. Finished multi-layer glass panel gives a double benefit: safety and control of radiation transmission.
[0004] An optical quality defect that can be particularly noticeable when viewed from an oblique angle can occur in such glass protective panels as a visible, isotropic reflection image resembling a wave with an estimated amplitude of about 0.002 to 0.012 mm and a wavelength of 2.5 - 7, 5 mm. It is further referred to as "appleauce" (apple puree). The probable reason for this phenomenon is that the polyethylene type layer, which reflects light when viewed at an oblique angle, adapts to the poly (vinyl butyral) type layer during lamination and takes over any non-linearity or waviness that occurs on such poly (vinyl butyral) layer . Other undesirable visual defects, such as "spots" (mottled), may also occur in colored poly (vinyl butyral) laminates if poly (vinyl butyral) layers are in contact with each other. For example, mottling may occur when pigmented poly (vinyl butyral) is extruded together with non-pigmented poly (vinyl butyral), and the obtained layer is then laminated with other layers or glass.
[0005] Several attempts have been described to reduce the severity of "applesauce" and mottling (see, for example, US Patent Nos. 4,465,736, 4,973,511 and 5,091,258), but further methods are needed to reduce "appleauce" and mottling. Therefore, improved compositions and methods of improvement are needed
The characteristics of polymer and poly (vinyl butyral) sheets that are used in conjunction with a polymer film layer, in particular polyethylene terephthalate, without adversely affecting the optical characteristics of the resulting multilayer structure.
SUMMARY OF THE INVENTION [0006] At present, polymer sheets have been developed in accordance with the present invention, which prior to laminating have low waviness and high roughness, which allows the production of multilayer laminated glass panels with low distortion containing poly (ethylene terephthalate) layers, or multilayer laminated glass panels with low distortion containing adjacent layers of poly (vinyl butyral) material.
[0007] The present invention includes a polymer sheet comprising: poly (vinyl butyral) and a plasticizer, wherein the polymer sheet has a surface with a waviness index less than 20,000 square microns, R value<sub>from</sub> is at least 20 micrometres and durability between 10 and 95.
[0008] The present invention includes a method of producing a multilayer intermediate layer comprising the steps of: forming a first polymer sheet comprising poly (vinyl butyral) and a plasticizer, said first polymer sheet having a first surface and a second surface, said first surface having a waviness index less than 20,000 square microns, value of R<sub>from</sub> at least 20 microns and durability between 10 and 95; placing the polymer film layer in contact with said first layer of said first polymer sheet to form a stack and laminating said stack.
[0009] The present invention includes a production method comprising forming a layer comprising poly (vinyl butyral) and a plasticizer, said layer having a first surface and a second surface and a waviness index less than 20,000 square micrometres, R value<sub>from</sub> at least 20 microns on said first surface, and extruding said layer on said first surface using a template having a specified roughness, resulting in said polymer sheet, said polymer sheet having a waviness factor less than 20,000 square microns and an R value<sub>from</sub> at least 20 microns on the side corresponding to said first surface of said layer.
[0010] The present invention includes a method of making a multilayer panel comprising the steps of: forming a first polymer sheet comprising poly (vinyl butyral) and a plasticizer, said first polymer sheet having a first surface and a second surface, said first surface having a waviness factor less than 20,000 square micrometres, an R2 value of at least 20 micrometres and a durability of 10 to 95, placing the polymer film layer in contact with said first layer of said first polymer sheet to form a stack, arranging the glass layer in contact with said polymer sheet facing said polymer film, and laminating said stack.
EP 1 874 535 B1
BRIEF DESCRIPTION OF THE DRAWINGS [0011]
Figure 1 is a schematic illustration of the construction of a laminated polymer sheet / polymer film.
DETAILED DESCRIPTION [0012] In accordance with the present invention, it has been discovered that a defect known as "applesauce" that can occur in multilayer glass panels containing a poly (vinyl butyral) sheet in contact with a layer of polymer film such as poly (ethylene terephthalate) can be reduced by using the polymer sheet and / or methods of the present invention. Furthermore, the mottling effect can be similarly reduced. The polymer sheets of the present invention have a low waviness index (WI), which is a measure of the waviness of the sheet surface, and a high roughness value (R<sub>from</sub>), which is a measure of smaller irregularities that usually occur on the surface of the sheet and are desirable.
[0013] As shown in Figure 1, generally at item 10, some embodiments of the present invention include the reduction of distortion that may occur due to the existence of the interlayer 12 between the polymer sheet 14 and the polymer film layer 16. As will be described in more detail below, the polymer sheet 14 it may contain a poly (vinyl butyral) material, and the polymer film layer 16 may include a poly (ethylene terephthalate) material. Typically, the multilayer glass panel may comprise a polymer sheet 14 and the polymer film layer 16 shown in Figure 1, as well as a second layer of the polymer sheet (not shown) in contact with the polymer film layer 16 on the opposite side of the polymer sheet 14. This three-layer construction may then found between two layers of glass forming a multi-layer glass panel.
[0014] The production of the polymer sheet of the present invention involves the production of a polymer sheet with low waviness index and high roughness. The low waviness factor of polymer sheet 14 reduces the occurrence of "applesauce" and / or mottling in the finished glass panel by reducing the distortion at the contact point 12 between the polymer sheet 14 and the polymer film layer 16 or between two layers of the polymer sheet (not shown), while the high roughness enables proper deaeration of layers during lamination. In various embodiments of the present invention, one or both surfaces of the polymer sheet may have a low waviness index and a high roughness value.
[0015] The present invention includes polymer sheets that have been prepared by the method of the present invention. The present invention includes methods for producing a polymer sheet that consists of the steps of making a polymer sheet having a surface with a low waviness index and a low roughness value, and extruding such a polymer sheet surface to impart high roughness.
[0016] Earlier attempts to reduce or eliminate "applesauce" consisted, inter alia, in the production of a softened poly (vinyl butyral) layer with a low waviness index. Such attempts often led to layers lacking the desired properties because of their value
The roughness of the resulting smooth layer was low, which caused difficulties in the lamination stages of the assembly process. Other attempts to reduce applesauce included a method in which a polymer film layer, such as polyethylene terephthalate, was sandwiched between two poly (vinyl butyral) layers rolled to form a three-layer laminate and then extruded on the exposed surface of poly (vinyl butyral) layers (see Japanese Patent Application JP59223256). Lamination of smooth poly (vinyl butyral) poly (ethylene terephthalate) can cause difficulties at the bleeding stage of the lamination process.
[0017] The present invention provides a method of producing a polymer sheet with a low waviness index and a high roughness value, resulting in a reduction or elimination of "applesauce" and other optical defects that may occur when the polymer film is used in combination with a polymer sheet, such such as poly (vinyl butyral), or defects that may occur when multiple layers of poly (vinyl butyral) are used.
[0018] In a first step of individual embodiments of the present invention, a polymer sheet is produced that has on one or both surfaces not necessarily the same waviness factor less than 20,000 square micrometres, less than 15,000 square micrometres, less than 12,000 square micrometres, less than 10,000 square micrometers , smaller than 8,000 square microns, less than 6,000 square microns or less than 5,000 square microns and a roughness value less than 15 microns, less than 12 microns, less than 10 microns, less than 9 microns, less than 8 microns, less than 7 microns, less than 6 microns or less than 5 micrometres, and the values given above for the waviness index and roughness values can be combined in any combination. In particular specific embodiments of the present invention, WI and R<sub>from</sub> are less than 20,000 micrometres and smaller than 20 micrometers, smaller than 15,000 square micrometers and smaller than 10 micrometers, smaller than 15,000 square micrometers and smaller than 7 micrometers, or are smaller than 15,000 square micrometers and smaller than 5 micrometers. The values given in this paragraph are the values of waviness and roughness before extrusion.
[0019] In the next step of these implementations, the relatively smooth surface or surfaces are extruded with a template having a certain roughness. This template can be any suitable template, which in individual implementations allows to obtain a polymer sheet with a final roughness value (value after extrusion) at least 20 microns, at least 25 microns, at least 30 microns, at least 35 microns, at least 45 microns, or at least 55 microns. Because this extrusion step is carried out before laminating the poly (ethylene terephthalate) layer or glass or other poly (vinyl butyral) layer, the extruded surfaces allow better venting between the layers of the final product.
[0020] By using the methods of the present invention, it has been discovered that it is possible to produce polymer sheets having one or both surfaces with preferably a low waviness index and a relatively high roughness value. In particular, in individual embodiments of the present invention, the polymer sheet after extrusion with a rough pattern has a waviness factor less than 20,000 square microns, less than 15,000 square microns, less
EP 1 874 535 B1 than 12,000 square microns, less than 10,000 square microns, less than 8,000 square microns, less than 6,000 square microns or less than 5,000 square microns, and a roughness value of at least 20 microns, at least 25 microns, at least 30 microns , at least 35 microns, at least 45 microns or at least 55 microns, the above values for the waviness index and roughness values can be combined in any combination as required. The values given in this paragraph are the values of corrugation and roughness after extrusion. For these and other embodiments of the present invention in which both the WI and roughness value are given, the respective other embodiments are also part of the present invention, only the roughness values, and not the WI, which are used to characterize the polymer sheet are given.
[0021] In addition to WI and roughness values, the polymer sheets of the present invention are characterized by their durability, which is a measure of the variability of the subtle topography structure of the sheet surface. Determination of the durability of one or both surfaces of the polymer sheet can be performed according to the procedure described elsewhere in the document.
[0022] The polymer sheets of the present invention, which are made to obtain low roughness and corrugation and extruded to a high roughness value, can have durability values in the range of 95-10. This range contrasts with polymer sheets that are based only at the turn of the alloy to obtaining surface roughness, which generally have durability values of 100 or close to 100. The durability value given to the polymer sheet will depend on the particular application and lamination conditions. For applications where maximum reduction of "applesauce" is desired, for example, the polymer sheets of the present invention may have durability values less than 40, less than 30 or less than 20, which does not mean that "applesauce" is not reduced in other projects with higher durability values. In other embodiments where it is desirable to reduce other defects, the polymer sheet may be given durability values from 60 to 95, 65 to 90, or 70 to 80. Other durability values that are useful in particular embodiments of the present invention are 10 to 30 , 30 to 50 and 50 to 95, 50 to 90 or 50 to 85.
[0023] The durability values given in this paragraph can be combined in any combination with the abovementioned roughness and corrugation values after extrusion.
[0024] The durability value of the polymer sheets of the present invention can be adjusted by varying, for example, each of the following parameters: a change in the pressure pressure of the pressure roller to press the material against the embossing and / or smoothing roller (s) to a higher pressure is associated with higher durability ; raising the surface temperature of the polymer by contact or non-contact methods, for example using infrared heaters, is associated with higher durability; changing the line speed to regulate the rate at which the polymer takes up heat: lower line speeds are associated with higher durability.
[0025] By changing the durability, the polymer sheet of the present invention can be adapted to be compatible with a specific manufacturing process. For example, a durability of 25 to 40 can be used for a process with pre-pressing with an outer roller, and a durability of 50 to 80 can be used for a process with pre-pressing with a vacuum bag.
[0026] The production of a polymer sheet that is sufficiently smooth to obtain the above-mentioned values prior to extrusion - that is, has a sufficiently low corrugation coefficient and a roughness value - can be obtained by changing the typical method of making the polymer sheet to the following.
[0027] For manufacturing methods in which a matrix is used to make the polymer sheet, an extremely smooth surface can be obtained by sufficiently increasing the temperature of the die edge to produce sheets having the aforementioned waviness index and roughness parameters prior to extrusion. In individual implementations, the matrix outlet temperature is maintained in the range of 170 ° C to 230 ° C, 190 ° C to 210 ° C or 195 ° C to 205 ° C.
[0028] For applications where a coating roll is used to form the polymer sheets, smoothness can be achieved by using a mirror-polished funnel roll, for example made of chromium, having no or low surface roughness or corrugation, and / or using high temperature blades. In other implementations, the mirror-polished funnel roller is used to achieve the same effect. Generally, the waviness of the sheet produced will be similar to the waviness of the coating roll surface, so the waviness of the coating roll should be maintained in accordance with the desired waviness of the finished sheet. Of course, the person skilled in the art will know that the production parameters used will depend on the molten polymer used and the equipment that is used to make the polymer sheet, but that the corresponding smoothness according to the present invention can easily be achieved by changing the production parameters as described herein.
[0029] The second step, which is embossing the roughness template on a smooth polymer sheet, can be performed by any suitable method, for example by using rollers having a roughness pattern, so that the reverse ("negative") image gives one or both surfaces of the polymer sheet. The result of this stage is to increase the roughness value to the desired high values. One or more additional rollers may be used between the sheet extrusion point and the individual process steps according to the desired control and forming of the sheets.
[0030] The present invention includes the following various embodiments:
[0031] In particular embodiments, the present invention includes a polymer sheet, such as polyvinyl butyral, having at least one surface having the above WI and Rz values after extrusion. The present invention further includes a polymer sheet, such as polyvinyl butyral, having two surfaces having the above WI and R values<sub>from</sub>after extrusion.
[0032] The present invention also includes a polymer sheet, such as poly (vinyl butyral), having one or both surfaces with the above WI and R values<sub>from</sub>after extrusion, the layer being not in contact with other layers, but rather being a single polymer sheet not embedded in any laminate.
[0033] In various embodiments, the present invention includes a multilayer intermediate layer for use in laminated glass, the intermediate layer comprising a polymer sheet, such as poly (vinyl butyral), which prior to laminating the surface to a polymer film, such as polyethylene terephthalate, has area with the above WI and R values<sub>from</sub>after extrusion.
[0034] The present invention includes a polymer sheet or multilayer intermediate layer comprising a polymer sheet or polymer film made in one of the processes of the present invention.
In various embodiments, the present invention includes a method of making a multilayer glass panel, comprising stacking the polymer sheet of the present invention with one or more polymer films or polymer sheets and forming an intermediate layer.
[0036] In various embodiments, the present invention includes a method of making a multilayer glass laminate, comprising stacking the polymer sheet of the present invention with one or more polymer films or polymer sheets forming an intermediate layer, and then forming the multilayer glass panel by laminating the intermediate layer between two layers of glass. These panels can be a type of laminated glass structure, including, without limitation, building glass and vehicle windshields.
In various embodiments, the present invention includes a windshield or window comprising one of the polymer sheets or intermediate layers in accordance with the present invention.
[0038] In various embodiments, the present invention includes a method of producing a multilayer intermediate layer, comprising forming a polymer sheet in which both surfaces of the polymer sheet have the values given above for extrusion, the extrusion of the polymer sheet on one or two surfaces, whereby the extrusion results in a surface having the values given after extrusion, and laminating the polymer sheet to the polymer film, wherein the polymer film is applied to the extruded surface of the polymer sheet.
[0039] Other embodiments include laminating a polymer film between two polymer sheets, wherein the present invention is brought to contact one or both surfaces of the polymer sheets with a polymer film. Further implementations include laminating the above-described three-layer intermediate layer between two layers of glass. As a further example, some implementations may have more than one polymer film, for example the following construction: polymer sheet // polymer film // polymer sheet // polymer film // polymer sheet.
[0040] In another embodiment, a structure having the glass // polymer sheet // polymer film system can be formed first by laminating the polymer sheet and polymer film, and then laminating this combination to glass or by laminating all three simultaneously. Any of the polymer sheets of the present invention may be used in this embodiment. In conventional applications where this three-layer system is used, the polymer film layer, which is typically polyethylene terephthalate, is typically thicker than the polymer films used in glass // sheet // film // sheet // glass realizations. This additional thickness is usually required to obtain a stiffer film, resistant to deformation and consequently optical defects that occur when a second rigid glass plate is not used to support the polymer layers. In embodiments of the present invention comprising a glass layer, a polymer sheet of the present invention and a polymer film, a relatively thinner polymer film can be used in the resulting three-layer structure, because the better quality of the polymer sheets of the present invention allows for a better reduction of optical defects.
[0041] The present invention can be used to reduce a defect known as gradient mottling. Gradient mottling is a defect observed in windshields made of gradient poly (vinyl butyral) and similar polymers in which dark colored poly (vinyl butyral) is coextruded in a layer of transparent poly (vinyl butyral). The gradient (shaded) part of the windshield may show patchy dark and light areas. In some products, windshields also contain a film of polyethylene terephthalate for protection from the sun. In this case, gradient mottling and applesauce can occur simultaneously.
[0042] In applications where pigments, dyes or other means are used to create a darkened area within the windshield, for example, the production of a polymer sheet using the methods of the present invention allows to obtain in various embodiments a product with the values given above before and after extrusion. Subsequent lamination of the polymer sheet having a gradient in the glass laminate, with or without other layers, results in a reduction of gradient mottling. Accordingly, the present invention includes embodiments in which a colored gradient polymer sheet is produced by the methods of the present invention, and multi-layer glass panels containing polymer sheets are also produced in this manner.
[0043] Further implementations reduce LAG mottling that may appear in colored building laminates made of layers of transparent or colored poly (vinyl butyral) in contact with each other. LAG mottling has an appearance similar to gradient mottling. Various embodiments of the present invention include multilayer building glass panels comprising multilayer polymer sheets. These embodiments of the present invention include methods for making multi-layer polymer sheet constructions in which two or more polymer sheets, of which at least one is produced by the method of the present invention, are in contact with each other and optionally with a layer of polymer film such as polyethylene terephthalate ) and a layer of glass, and then they are laminated into a finished product. These implementations include two poly (vinyl butyral) polymer sheets that are laminated in contact with each other, wherein one or both polymer sheets may have one or both surfaces with pre and post extrusion values given elsewhere in the document, and one or both sheets polymeric may contain a dye. In other embodiments, the polymer sheet of the present invention is in contact with another polymer sheet and none of the polymer sheets contain pigment or dye.
POLYMER FILM [0044] The polymer film layer 16 shown in Figure 1 can be any suitable thermoplastic film that is customarily used as a performance enhancing layer in multilayer glass panels. In various embodiments, the polymer film layer 16 has a thickness of 0.013 mm to 0.20 mm, preferably 0.025 mm to 0.1 mm, or 0.04 to 0.06 mm. The polymer film layer 16 may optionally be a treated or coated surface to improve one or more properties, such as adhesion or reflection of infrared radiation. These functional performance enhancing layers include, for example, a multilayer stack reflecting infrared radiation and transmitting visible light when exposed to sunlight. Such a multilayer stack is known in the art (see, for example, WO 88/01230 and US Patent 4,799,745) and
EP 1 874 535 B1 may comprise, for example, one or more metallic layers of angstrom thickness and one or more (e.g. two) applied successively, optically cooperating dielectric layers. As is also known (see, for example, US Pat. Nos. 4,017,661 and 4,786,783), the metal layer or layers may optionally be electrically heated to defrost or remove fog from the combined glass layers.
[0045] The polymer film layer 16 in some implementations is optically transparent (i.e., objects on one side of the layer can be seen from the other side of the layer without obstacles) and usually has a larger, in some embodiments significantly larger, stretching module regardless of the composition of the adjacent polymer sheet 14. In various embodiments, the polymer film layer 16 comprises a thermoplastic material. Thermoplastic materials with suitable properties include nylons, polyurethanes, acrylic materials, polycarbonates, polyolefins such as polypropylene, cellulose acetates and triacetates, vinyl chloride polymers, copolymers, etc. In various implementations, the polymer film layer 16 includes materials such as re-stretched thermoplastic films having the aforementioned properties, which include polyesters, e.g., poly (ethylene terephthalate) and poly (ethylene terephthalate) glycol (PETG). Polyethylene terephthalate is used in various implementations and poly (ethylene terephthalate) is biaxially stretched to improve strength and stabilized in heat in order to achieve low shrinkage in the event of elevated temperature (e.g. less than 2% shrinkage in both directions) after 30 minutes at 150 ° C).
[0046] Various coatings and surface treatment techniques for polyethylene terephthalate film that can be used in the present invention are disclosed in published European Application No. 0157030. POLYMER SHEET [0047] The following section describes various materials that can be used to form the polymer sheets of the present invention, shown as item 14 in Figure 1, which have properties useful as an intermediate layer in safety glass, such as poly (vinyl butyral).
[0048] The term "polymer sheet" as used herein means a polymer composition formed in any suitable manner into a thin layer that is suitable for use as an intermediate layer in laminated glass materials. The term "resin" as used herein refers to a polymer component (e.g., poly (vinyl butyral)) that is removed from the mixture resulting from acid catalysis and subsequent neutralization of polymer precursors. The resin usually has, in addition to a polymer, e.g. poly (vinyl butyral), other ingredients such as acetates, salts and alcohols. The term "alloy" as used herein refers to a molten mixture of resin with plasticizers and optionally other additives.
[0049] Polymer sheets made in the process described herein form part of the present invention and are included within its scope.
[0050] The polymer sheets of the present invention may contain any suitable polymer, and in a preferred embodiment, as illustrated above, the polymer sheet comprises poly (vinyl butyral). In some embodiments of the present invention given herein that comprise poly (vinyl butyral) as the polymer component of the polymer sheet, another embodiment is contemplated wherein the polymer component consists of or consists essentially of poly (vinyl butyral). In these implementations, the additions can be changed freely, in
The plasticizers described herein, and used with a polymer sheet containing a polymer consisting of or consisting essentially of poly (vinyl butyral).
[0051] In one embodiment, the polymer sheet comprises a polymer based in part on acetalated poly (vinyl alcohols). In another embodiment, the polymer sheet comprises a polymer selected from the group consisting of poly (vinyl butyral), polyurethane, poly (vinyl chloride), ethylene vinyl acetate copolymer, combinations thereof, etc. In one embodiment, the polymer sheet comprises poly (vinyl butyral). In other embodiments, the polymer sheet comprises plasticized poly (vinyl butyral). In further embodiments, the polymer sheet comprises poly (vinyl butyral) and one or more other polymers. Other polymers having an appropriate glass transition temperature may also be used. In the parts of the document in which the preferred ranges, values and / or methods are given specifically for poly (vinyl butyral) (for example, and without limitation, in the case of plasticizers: component percentage, thickness and characteristics of additives improving properties), these ranges also apply , if applicable, for other polymers and polymer blends provided herein as useful constituents of polymer sheets.
[0052] For implementations containing poly (vinyl butyral), poly (vinyl butyral) can be produced by a known acetalation process that involves the reaction of polyvinyl alcohol (PVOH) with butyraldehyde in the presence of an acid catalyst followed by neutralization of the catalyst, separation, stabilization and drying of the resin .
[0053] In various embodiments, the polymer sheet containing poly (vinyl butyral) contains 10 to 35 percent by weight (wt.%) Of hydroxyl groups based on polyvinyl alcohol, 13 to 30 wt. hydroxyl groups based on polyvinyl alcohol or 15 to 22 wt. hydroxyl groups expressed as polyvinyl alcohol. The polymer sheet may also contain less than 15 wt. residual ester groups of 13% by weight, 11% by weight, 9% by weight, 7% by weight, 5% by weight or less than 3 wt. residual ester groups expressed as polyvinyl acetate, with a predominance of acetal, preferably butyraldehyde acetal, but possibly containing smaller amounts of acetal groups, e.g. 2-ethylhexanal (see, for example, US Patent 5,137,954).
[0054] In various embodiments, the polymer sheet comprises a poly (vinyl butyral) having a molecular weight of at least 30,000, 40,000, 50,000, 55,000, 60,000, 65,000, 70,000, 120,000, 250,000 or at least 350,000 grams per mole (g / mole or dalton). During the acetalation step, small amounts of dialdehyde or trialdehyde can also be added to increase the molecular weight to at least 350 g / m (see, for example, US Patent 4,902,464; 4,874,814; 4,814,529; 4,654,179). The term "molecular weight" as used herein means a weighted average molecular weight. Any suitable method can be used to make the polymer sheets of the present invention. Details of suitable processes for making poly (vinyl butyral) are known to those skilled in the art (see, for example, US Patent Nos. 2,282,057 and 2,282,026). In one embodiment, the solvent method described in Vinyl Acetal Polymers, Encyclopedia of Polymer Science & Technology, 3rd Edition, Volume 8, pages 381-399, BE Wade (2003) can be used. In another embodiment, the aqueous method described therein may be used. Poly (vinyl butyral) is commercially available in various forms, for example from Solutia Inc., St. Louis, Missouri as Butvar ™ resin.
[0055] Various adhesion regulating substances can be used in the polymer sheets of the present invention, such as sodium acetate, potassium acetate and magnesium salts. Magnesium salts that can be used in these embodiments of the present invention include, but are not limited to, those in U.S. Patent 5,728,472, such as magnesium salicylate, magnesium nicotinate, magnesium di- (2-aminobenzoate), di- (3-hydroxy-2- magnesium naphthalene carboxylate, and magnesium bis (2-ethylbutyrate) (Chemical Abstracts registry number 79992-76-0). In particular embodiments of the present invention, the magnesium salt is magnesium bis (2-ethylbutyrate).
[0056] Additives may be incorporated into the polymer sheet to improve the properties of the finished product. Such additives include, but are not limited to, plasticizers, dyes, stabilizers (e.g., ultraviolet stabilizers), antioxidants, anti-blocking agents, flame retardants, IR absorbers, combinations of the above additives and the like known in the art.
[0057] In particular embodiments of the polymer sheets of the present invention, the polymer sheets may contain 20 to 60, 25 to 60, 20 to 80 or 10 to 70 parts of plasticizer per hundred parts of resin (phr). Of course, other amounts may be used if appropriate for the particular application. In some embodiments, the plasticizer has a hydrocarbon segment having less than 20, less than 15, less than 12 or less than 10 carbon atoms.
[0058] The amount of plasticizer can be adjusted to change the glass transition temperature (Tg) of the poly (vinyl butyral) sheet. Higher amounts of plasticizer are usually added to reduce the Tg. The poly (vinyl butyral) polymer sheets of the present invention may have a Tg value of 40 ° C or less, 35 ° C or less, 30 ° C or less, 25 ° C or less, 20 ° C or less, or 15 ° C or less.
[0059] In the production of the polymer sheets of the present invention, any suitable plasticizers can be added to the polymer resins. The plasticizers used in the polymer sheets of the present invention may be, among others, esters of a polybasic acid or polyhydric alcohol. Suitable plasticizers are, for example, triethylene glycol di- (2-ethylbutyrate), triethylene glycol bis (2-ethylhexanoate), triethylene glycol diheptanoate, tetraethylene glycol diheptanoate, dihexyl adipate, dioctyl adipate, cyclohexyl adipate adipine heparinate diisononyl, heptylononyl adipate, dibutyl sebacate, polymer plasticizers, such as modified oil sebacate alkyds and a mixture of phosphates and adipates as described in U.S. Patent No. 3,841,890, and adipates as described in U.S. Patent No. 4,144,217 and mixtures or combinations given previously. Other plasticizers that can be used are mixed adipates obtained from C4 to C9 alkyl alcohols and C4 to C10 cycloalcohols as described in US Pat. No. 5,013,779, and C6 to C8 adipate esters such as hexyl adipate. In some embodiments, the plasticizer is triethylene glycol bis (2-ethylhexanoate).
[0060] The poly (vinyl butyral) polymer and plasticizing additives can be thermally processed and formed into sheets by methods known to those skilled in the art with the method modifications described above to form a polymer sheet with the desired waviness index and roughness value before stamping. One example of forming a poly (vinyl butyral) sheet is extrusion of molten poly (vinyl butyral) containing resin, plasticizers and additives (referred to herein as "alloy") by
A die (e.g., a die having an opening that is significantly larger in one dimension than in the perpendicular dimension). Another exemplary method of forming a poly (vinyl butyral) sheet involves pouring the melt from a die onto a shaft, solidifying the resin, and then removing the solid resin as a sheet. In various embodiments, the polymer sheets can be 0.1 to 2.5 millimeters thick, 0.2 to 2.0 millimeters, 0.25 to 1.75 millimeters, and 0.3 to 1.5 millimeters (mm).
[0061] The present invention also includes the stacks or rolls of any of the polymer sheets of the present invention disclosed herein in any combination as described herein.
[0062] In addition, the present invention includes laminated safety glass comprising a layer of glass, usually consisting of silicon dioxide, in contact with any of the polymer / polymer film sheet embodiments of the present invention. Furthermore, the invention includes laminated safety glass comprising two glass sheets with any polymer sheet / polymer film according to the present invention in between.
[0063] The present invention also includes windshields, windows and other finished glass products comprising the multilayer structures of the present invention.
[0064] Various characteristics of the polymer sheet and / or laminated glass as well as measuring techniques used in the context of the present invention are described below.
[0065] As used herein, the values "waviness index" or "WT" and "roughness value" or "R<sub>from</sub>"Can be marked as follows:
[0066] To determine R<sub>from</sub> a test sample of 15 cm x 15 cm plasticized polymer sheet is placed on a vacuum plate controlled by the liquid flowing through it at room temperature. A 5 psi vacuum is applied to press the sample against the surface of the plate. For direct measurement of the sheet surface roughness on each side of the test sample, a Perthometer model S&P with PRK drive unit and RFHTB-250 measuring needle (available from Mahr Gage Co., New York) are used. The profile selection is set to "R" on the instrument. The measuring needle automatically moves across the surface of the sample. The length of each measurement is 17.5 mm, which consists of 7 consecutive lengths L0 of 2.5 mm. The measuring section is 12.5 mm and consists of 5 measuring sections obtained by excluding the first and last sections. The average value of individual roughness values Lc in these five consecutive measuring sections is determined, while R<sub>from</sub> is the average of ten determinations, five in the extrusion direction of the device (MD) and five in the transverse direction of the device (CMD). The distance between two successive paths in each direction is 3 mm.
[0067] In order to determine the value of the waviness index (WI), the Perthometer profile previously mentioned is used with the profile selection set to "W". For this measurement, a measuring length of 56 mm and a measuring distance of 40 mm are used.
[0068] The 40 mm measuring section consists of five 8 mm sections (two end 8 mm measuring sections are excluded). Using the digital output from the plug connector on the back of the profilometer, the variable wave output voltage signal from the profilometer is sent electronically to the computer. Ten measurements are made, five in the extrusion direction of the device and five in the direction transverse to
EP 1 874 535 B1 of the device, wherein the distance between two consecutive measurements is 3 mm. The Sub SmoothDataO program, installed on the computer and attached to this one, calculates a single WI value from the input data for ten measurements.
[0069] The WI value of the surface of the polymer sheet, for example from a sheet that is formed for use in a windshield, is then calculated by averaging 100 individual WI values from evenly distributed measuring points over the entire sheet surface.
[0070] The same calculations can be made for the opposite surface and, as described elsewhere in the document, similar or different results can be obtained depending on the method of manufacture and the desired product. In particular embodiments of the present invention, at least 90 of the 100 values obtained were within the range of +/- 20% average of 100 values, +/- 15% average, +/- 10% average, +/- 5% average, or + / -2% average of 100 values. Unless otherwise indicated in the patent claim, when the "WI value" for the surface of the polymer sheet is given in the patent claim, at least 90 of the 100 values obtained in the measurement process described above was within +/- 20% of the average of 100 values.
[0071] Using the above-mentioned Perthometer profilometer, the other switch position settings for roughness are as follows: Filter: GS, Profile: R, LC: N 2.5 mm, LT: 17.5 mm, VB: 625 micrometers. The settings for waviness are as follows: Filter: GS, Profile: W, LC: N 8.0 mm, LT: 56 mm, VB: 625 microns.
[0072] The polymer sheets of the present invention are also characterized by their "stability", which is determined as follows: for polymer sheets that are extruded, the polymer sheet is measured before extrusion to obtain an R value<sub>from</sub> (R<sub>from</sub> reference). After extrusion, a second R measurement is made<sub>from</sub> (R<sub>from</sub> final). For polymer sheets that are not extruded, a roughness measurement is taken, R<sub>from</sub>and denotes it as R<sub>from</sub> final values and R values<sub>from</sub> reference is set to zero. Then for both extruded and non-extruded sheets<sub>2</sub> polymer cut out sample with an area of 12.7 cm<sup>2</sup>. A piece of polyethylene terephthalate with an area of 14<sub>2</sub> cm<sup>2</sup> is placed on a wooden frame, laying it on a horizontal surface, the periphery of the frame is slightly smaller than the sample of the polymer sheet. Then a sample of the polymer sheet is placed on the polyethylene terephthalate film, and then another portion of the polyethylene terephthalate film is placed on the polymer sheet. A second frame is then placed on top of the polymer layers. The frames are then compressed together with clips. The frame and polymer assembly is then placed in a preheated oven for 5 minutes at 100 ° C. The set is then removed and allowed to cool. Then the second R value is determined<sub>from</sub>for a polymer sheet sample (R<sub>from</sub> 100 ° C).
[0073] Then the durability can be determined according to the following formula:
Persistence = [(R<sub>from</sub> 100<sup>about</sup>C -R<sub>from</sub> Reference) / (R<sub>from</sub> final - R<sub>from</sub> references)] * 100 [0074] The transparency of the polymer sheet, and especially the poly (vinyl butyral) sheet, can be determined by measuring the haze value, which is a quantitative assessment of the light not transmitted through the sheet. The haze percentage can be measured as follows. Hazemeter, Model D25 Haze Meter, which can be obtained from Hunter Associates (Reston, VA), can be used in accordance with ASTM
D1003-61 (Procedure A, re-approved in 1977) using lighting C and observing
EP 1 874 535 B1 at an angle of 2 degrees. In particular embodiments of the present invention, the haze percentage is less than 5%, less than 3%, and less than 1%.
[0075] Pummel adhesion can be measured in the following manner, wherein "impact" here refers to the quantification of the adhesion of the polymer sheet to glass; the following technique is used to determine the impact. Two-layer glass laminate samples are prepared under standard autoclave lamination conditions. The laminates are cooled to about -17 ° C (0 ° F) and broken by hand with a hammer to break the glass. Then, all the glass that does not adhere to the poly (vinyl butyral) sheet is removed, and the amount of remaining glass adhering to the poly (vinyl butyral) sheet is compared visually with the set of standards. These standards correspond to the scale at which the glass remains adjacent to the poly (vinyl butyral) sheet to varying degrees. In particular for the zero pattern, the glass does not remain adjacent to the poly (vinyl butyral) sheet at all. In the 10 standard, 100% glass remains adjacent to the poly (vinyl butyral) sheet. In the case of laminated glass panels according to the present invention, different embodiments have an impact strength of at least 3, at least 5, at least 8, at least 9 or 10. Other embodiments have a value between 8 and 10 inclusive.
[0076] The "yellowness index" of the polymer sheet can be measured as follows: transparent 1 cm thick polymer sheet discs are formed having smooth surfaces that are substantially flat and parallel. The ratio is measured by ASTM D 1925, Standard Test Method For Yellowness Index of Plastics spectrophotometrically based on visible light transmitted. The values are corrected to a thickness of 1 cm based on the measured thickness of the sample. In various embodiments, the yellowness index is less than 0.6, 0.5 or 0.25.
Example 1 [0077] The first multilayer glass panel is formed from the following layers: glass // poly (vinyl butyral) // poly (ethylene terephthalate) // poly (vinyl butyral) // glass, where poly (ethylene terephthalate) is 0.05 mm Dupont Mylar®, and poly (vinyl butyral) layers are 0.38 millimeters thick and are made using conventional techniques.
[0078] The second multilayer glass panel is formed from the following layers: glass // poly (vinyl butyral) // poly (ethylene terephthalate) // poly (vinyl butyral) // glass, where poly (ethylene terephthalate) is 0.05 mm Dupont Mylar ®, and the poly (vinyl butyral) layers are 0.38 millimeters thick, and are made according to the present invention.
[0079] Subjective analysis of these two multilayer glass panels shows that the first panel has the visible "applesauce" when it is not present in the second panel.
Example 2 [0080] A 0.76 millimeter poly (vinyl butyral) sheet (first sheet) is co-extruded with a blue pigment. The sheet has WI = 13,000 and R<sub>from</sub>= 15 microns. This sheet is extruded up to 40 microns R<sub>from</sub>and WI = 16.000. This sheet is then laminated between two glass panes.
[0081] The second poly (vinyl butyral) sheet is produced by a conventional method and has a thickness of 0.76 millimeters and an R value<sub>from</sub>= 35. This second sheet is also laminated between two glass panes.
[0082] The results indicate that the mottling is visible on the second sheet, but not visible on the first. The imaging software shows that the mottle value is 3.9 for the first sheet and 14.5 for the second.
[0083] Thanks to the present invention, it is now possible to obtain a poly (vinyl butyral) sheet and other polymer sheets with better optical properties when used in combination with various other polymer sheets. Applesauce and mottling problems can be reduced or eliminated using the methods, polymer sheets and multilayer constructions of the present invention.
[0084] It will further be understood that any ranges, values or characteristics given for a single component of the present invention may be used interchangeably with any of the ranges of values or characteristics given for any other components of the invention, where appropriate, to achieve embodiments having values determined for each of the ingredients as specified in the document. For example, a polymer sheet having surface topography in any ranges can be formed along with any ranges given for plasticizers to create a variety of combinations within the scope of the present invention.
[0085] The reference numbers of the drawings given in the abstract are for illustration only and cannot be understood as limiting the claimed invention to one particular embodiment shown in the drawing. Drawings are not to scale unless otherwise indicated.
<td>Variable</td><td>Definition</td><td>Value</td>
<td>M</td><td>Minimal change in counting distance as vertices and valleys (in terms of number of points)</td><td>57.5 (changes according to the number of data points on each track)</td>
<td>L</td><td>Minimal altitude change to count as vertices and valleys</td><td> 5</td>
<td>NPTPT</td><td>Total number of data points in one track</td><td> 5760</td>
<td>NP</td><td>Number of vertices and valleys</td><td></td>
<td>FACT1</td><td>For converting data from Perthometer to microns</td><td> 0,038</td>
<td>FACT3</td><td>Coefficient for converting the number of points to mm</td><td>40 / NPTPT</td>
<td>NTraces</td><td>Number of Paths</td><td> 10</td>
<td>PsubM</td><td>Average stroke</td><td></td>
<td>PsubS</td><td>Standard deviation for the stroke</td><td></td>
<td>HsubM</td><td>medium height</td><td></td>
<td>HsubS</td><td>Standard deviation for height</td><td></td>
<td>RIPm</td><td>The average average jump for 10 tracks</td><td></td>
<td>Rihm</td><td>Average average height for 10 paths</td><td></td>
<td>WvIdx</td><td>Wave factor / 1000</td><td></td>
EP 1 874 535 B1
Sub SmoothDataO [0086]
1550 Rem Filter traces and Calculate Hm and Pm 1555 RIPm = 0 'RlPm is Roll Average Pm 1560 RlHm = 0' RlHm is Roll Average Hm 1615 For i = 1 To NTraces
1620 E = 0
1625 For k = l This is l50
1630 VL (k) = 0 'VL is Valley Height
1635 PK (c) = 0 'PK is Peak Height
1640 F (k) = 0 'F is Sample Point Corresponding to Extreme
1645 Next k
1650 For j = 1 To NPTPT 'Status Bar Update (Events Log)
If j = Multiple * NPTPT / 10 Then
Per% = 10 * (i -1) + ((j * 10) / NPTPT)
If Per%> 100 Then Per% = 100 frmMainWave.sspProgressBar.FloodPercent = Per%
Multiple = Multiple + 1
If Multiple = 11 Then Multiple = 1
End if
1655 If j> 1 Then GoTo 1805 'If not First Point
1656 Code for First Point in Each Trace Only
1660 If a (i, j) = a (i, j +1) Then GoTo 1745
1665 If a (i, j)> a (i, j +1) Then GoTo 1705 'First point is a maximum
1670 Rem First Point is a Minimum
1675 Extr = 0'Extr = 0 for Minimum, Extr = 1 for Maximum
1680 E = E +1 'Sets First Extreme
1685 VL (E) = a (i, j) 'Sets Value of 1st Valley = a (i, j)
1690 Direction = 1 Direction (+1 is up / -1 is down)
1695 FP (i) = 0 'Sets First Point as Minimum
1700 GoTo 1735
1705 Rem First Point is a Maximum
1710 Extr = 1
1715 E = E + 1
1720 FP (i) = 1 'Sets First Point as a Maximum
1725 Direction = -1
1730 PK (E) = a (i, j)
1735 F (E) = j
1740 GoTo 2200 'Next j (Next Point)
EP 1 874 535 B1
<td></td><td> 1745</td><td>Rem First Point is the Same as the Second Point, so Check Next Point</td>
<td></td><td> 1746</td><td>EQP = 1</td>
<td> 10</td><td> 1750</td><td>If a (i, j) = a (i, j + EQP +1) Then GoTo 1790 'Points are still the same</td>
<td></td><td> 1755</td><td>If a (i, j)> a (i, j + EQP + 1) Then GoTo 1775 'First Points are Maxima</td>
<td> 5</td><td> 1760</td><td>Rem First Points are Minima</td>
<td></td><td> 1765</td><td>j = j + EQP</td>
<td></td><td> 1770</td><td>GoTo 1670 'Run Routine for Minimum First Point</td>
<td> 15</td><td> 1775</td><td>Rem First Points are Maxima</td>
<td></td><td> 1780</td><td>j = j + EQP <</td>
<td> 10</td><td> 1785</td><td>> GoTo 1705 'Run Routine for Maximum First Point</td>
<td></td><td> 1790</td><td>Rem Points are Still the Same, Check Next point</td>
<td></td><td> 1791</td><td>EQP = EQP + 1</td>
<td> 20</td><td> 1795</td><td>If EQP = NPTPT -1 Then GoTo 2570 'Next i</td>
<td></td><td> 1800</td><td>GoTo 1750 'Check Next Point</td>
<td> 15</td><td> 1805</td><td>Rem This Section for Points After 1</td>
<td></td><td> 1810</td><td>EQP = 0</td>
<td></td><td> 1815</td><td>EP = j -l 25</td>
<td></td><td> 1820</td><td>If a (i, j) = a (i, j - 1) Then GoTo 2135 'Same Points</td>
<td></td><td> 1825</td><td>If a (i, j) <a (i, j - 1) Then GoTo 1985 'Falling Points</td>
<td> 20</td><td> 1830</td><td>Rem Rising Points</td>
<td></td><td> 1835</td><td>If Direction = 1 Then GoTo 2200</td>
<td></td><td> 1840</td><td>Rem Local Minimum Detected at Point EP (Extreme Point = j- 1 + CINT (EQP / 2)</td>
<td> 30</td><td> 1845</td><td>If Extr = 1 Then GoTo 1895 'Last Point was a Peak</td>
<td></td><td> 1850</td><td>Rem Last Extreme was a Valley</td>
<td> 25</td><td> 1855</td><td>If a (i, j) <= VL (E) Then GoTo 1870 'Current Valley was not a Valley</td>
<td></td><td></td><td>'since it Did Not Follow a Peak</td>
<td></td><td></td><td>'But Followed a Local Max</td>
<td></td><td> 1860</td><td>GoTo 1975</td>
<td></td><td> 1870</td><td>Rem Replace Last Valley with this One</td>
<td> 30</td><td> 1875</td><td>VL (E) = a (i, EP)</td>
<td></td><td> 1880</td><td>Extr = 0</td>
<td> 5</td><td> 1885</td><td>F (E) = EP</td>
<td></td><td> 1890</td><td>GoTo 1975</td>
<td></td><td> 1895</td><td>Rem Last Extreme was a Peak</td>
<td> 35</td><td> 1900</td><td>If Abs (a (i, EP) - PK (E))> = 1 Then GoTo 1915</td>
<td></td><td> 1905</td><td>Rem Height from Peak to this Mm does not Meat L Filtering Criteria</td>
<td> 10</td><td> 1910</td><td>GoTo 1975</td>
<td></td><td> 1915</td><td>If (EP - F (E))> = M Then GoTo 1950 'Found a Valley - Record It</td>
<td></td><td> 1920</td><td>Rem Number of Points from peak to mis Min does not Meet</td>
<td> 40</td><td> 1925</td><td>Rem M Filtering Criteria</td>
EP 1 874 535 B1
<td></td><td> 1930</td><td>If E = 1 Then GoTo 2200 'Next j (Next Point)</td>
<td> 15</td><td> 1935</td><td>If a (i, EP)> = VL (E -1) Then GoTo 1975</td>
<td></td><td> 1940</td><td>E = E + 1</td>
<td></td><td> 1945</td><td>GoTo 1870</td>
<td> 5</td><td> 1950</td><td>Rem Found a Valley - Record It</td>
<td></td><td> 1955</td><td>E = E + 1</td>
<td> 20</td><td> 1960</td><td>F (E) = EP</td>
<td></td><td> 1965</td><td>VL (E) = a (i, EP)</td>
<td></td><td> 1970</td><td>Extr = 0</td>
<td> 10</td><td> 1975</td><td>Direction = 1</td>
<td></td><td> 1980</td><td>GoTo 2200 'Next j (Next Point)</td>
<td> 25</td><td> 1985</td><td>Rem Falling Points</td>
<td></td><td> 1990</td><td>If Direction = -1 Then GoTo 2200 'Next j (Next Point)</td>
<td></td><td> 1995</td><td>Rem Local Max Detected at Point EP (Extreme Point = j-l + CINT (EQP / 2)</td>
<td> 15</td><td> 2000</td><td>If Extr = 0 Then GoTo 2045 'Last Extreme was a Valley</td>
<td></td><td> 2005</td><td>Rem Last Extreme was a Peak</td>
<td> 30</td><td> 2010</td><td>If a (i, EP)> = PK (E) Then GoTo 2020</td>
<td></td><td> 2015</td><td>GoTo 2125</td>
<td></td><td> 2020</td><td>Rem Replace Last Peak with This One</td>
<td> 20</td><td> 2025</td><td>PK (E) = a (i, EP)</td>
<td></td><td> 2030</td><td>Extr = 1</td>
<td></td><td> 2035</td><td>F (E) = EP</td>
<td></td><td> 2040</td><td>GoTo 2125</td>
<td></td><td> 2045</td><td>Rem L as Extreme was a Valley</td>
<td> 25</td><td> 2050</td><td>If Abs (a (i, EP) - VL (E))> = 1 Then GoTo 2065 'Pass L Filtering</td>
<td> 5</td><td> 2055</td><td>Rem Height from Valley to this Max does not Meet L Filtering Criteria</td>
<td></td><td> 2060</td><td>GoTo 2125</td>
<td></td><td> 2065</td><td>If (EP - F (E))> = M Then GoTo 2100 'Found a Peak - Record It</td>
<td></td><td> 2070</td><td>Rem Number of points from Valley to this max does NOT meet</td>
<td> 30</td><td> 2075</td><td>Rem M Filtering Criteria</td>
<td> 10</td><td> 2080</td><td>If E = 1 Then GoTo 2200 'Next j (Next Point)</td>
<td></td><td> 2085</td><td>If a (i, j) <= PK (E -1) Then GoTo 2125</td>
<td></td><td> 2090</td><td>E = E -l</td>
<td></td><td> 2095</td><td>GoTo 2020</td>
<td> 35</td><td> 2100</td><td>Rem Found as Peak - Record It</td>
<td> 15</td><td> 2105</td><td>E = E + 1</td>
<td></td><td> 2110</td><td>F (E) = EP</td>
<td></td><td> 2115</td><td>PK (E) = a (i, EP)</td>
<td></td><td> 2120</td><td>Extr = l</td>
<td> 40</td><td> 2125</td><td>Direction = -1</td>
EP 1 874 535 B1
<td></td><td> 20</td><td> 2130</td><td>GoTo 2200 'Next j (Next Point)</td>
<td></td><td></td><td> 2135</td><td>EQP = 1</td>
<td></td><td></td><td> 2140</td><td>If (j + EQP) <NPTPT Then GoTo 2155</td>
<td></td><td></td><td> 2145</td><td>j = NPTPT</td>
<td> 5</td><td></td><td> 2150</td><td>GoTo 2200 'Next j (Next Point)</td>
<td></td><td> 25</td><td> 2155</td><td>EP = j -1 + CInt (EQP / 2)</td>
<td></td><td></td><td> 2160</td><td>If a (i, j) = a (i, j + EQP) Then GoTo 2190</td>
<td></td><td></td><td> 2165</td><td>If a (i, j)> a (i, j + EQP) Then GoTo 2180</td>
<td></td><td></td><td> 2170</td><td>Rem Rising Points</td>
<td> 10</td><td></td><td> 2175</td><td>GoTo 1830</td>
<td></td><td> 30</td><td> 2180</td><td>Rem Falling Points</td>
<td></td><td></td><td> 2185</td><td>GoTo 1985</td>
<td></td><td></td><td> 2190</td><td>EQP = EQP +1</td>
<td></td><td></td><td> 2195</td><td>GoTo 2140</td>
<td> 15</td><td></td><td> 2200</td><td>Next j 'Next Point</td>
<td></td><td></td><td> 2205</td><td>NP = Int ((E - FP (i)) / 2) 'NP = # of Points</td>
<td></td><td></td><td> 2210</td><td>PsubM = 0 'PsubM = Pm = Mean Pitch</td>
<td></td><td></td><td> 2215</td><td>PsubS = 0 'PsubS = PS = Pitch Sigma (Std Dev)</td>
<td></td><td></td><td> 2220</td><td>HsubM = 0 'HsubM = Hm = Mean Height</td>
<td> 20</td><td> 5</td><td> 2225</td><td>HsubS = 0 'HsubS = Hs = Height Sigma (Std Dev)</td>
<td></td><td></td><td> 2230</td><td>Fact3 = 12.5 / NPTPT 'Fact3 Converts Point # Delta to 10<sup>Λ</sup>-3 meters</td>
<td></td><td></td><td> 2235</td><td>Fork = 1 To NP</td>
<td></td><td></td><td> 2240</td><td>P (k) = F (2 * k + I + FP (i)) - F (2 * k- 1 + FP (i))</td>
<td></td><td></td><td> 2245</td><td>If P (k)> 0Then GoTo 2260</td>
<td> 25</td><td> 10</td><td> 2250</td><td>NP = E.g. -1</td>
<td></td><td></td><td> 2255</td><td>GoTo 2275</td>
<td></td><td></td><td> 2260</td><td>PsubM = PsubM + P (k)</td>
<td></td><td></td><td> 2265</td><td>H (k) = PK (2 * k + FP (i)) - ((VL (2 * k + 1 + FP (i)) + VL (2 * k - 1 + FP (i))) / 2)</td>
<td></td><td></td><td> 2270</td><td>HsubM = HsubM + H (k)</td>
<td> 30</td><td> 15</td><td> 2275</td><td>Next k</td>
<td></td><td></td><td> 2280</td><td>PsubM = PsubM / NP</td>
<td></td><td></td><td> 2285</td><td>HsubM = HsubM / NP</td>
<td></td><td></td><td> 2290</td><td>DelPm = 0 'DelPm is the delta (X-Xbar)</td>
<td></td><td></td><td> 2295</td><td>DelHm = 0 'DelHm is the delta (X-Xbar)</td>
<td> 35</td><td> 20</td><td> 2300</td><td>DSqPm = 0 'DSqPm is the sum of delta squared (X-Xbar ^ 2</td>
<td></td><td></td><td> 2305</td><td>DSqHm = 0 'DSqHm is the sum of delta squared (X-Xbar ^ 2</td>
<td></td><td></td><td> 2310</td><td>For k = 1 To NP</td>
<td></td><td></td><td> 2315</td><td>DelPm = PsubM - P (k)</td>
<td></td><td></td><td> 2320</td><td>DSqPm = DSqPm + (DelPmΛ2)</td>
<td> 40</td><td> 25</td><td> 2325</td><td>DelHm = HsubM -H (k)</td>
<td></td><td></td><td> 2330</td><td>DSqHm = DSqHm + (DelHm Λ 2)</td>
EP 1 874 535 B1
<td></td><td colspan="2"> 2335</td><td>Next k</td>
<td></td><td></td><td></td><td>'Skip over an error which might occur in the calculation of the Std Dev</td>
<td></td><td> 30</td><td></td><td>On Error Resume Next</td>
<td></td><td></td><td> 2340</td><td>PsubS = Sqr (DSqPm / (E.g. -l))</td>
<td> 5</td><td></td><td> 2345</td><td>HsubS = Sqr (DSqHm / (NP -1)) 'Disable error checking On Error GoTo 0</td>
<td></td><td></td><td> 2355</td><td>Rem Convert H from Volts to Micro Meters</td>
<td></td><td> 5</td><td> 2359</td><td>Fact1 = 0.038 'Conversion factor for Volts to um (Taken from S8P documentation)</td>
<td> 10</td><td></td><td> 2360</td><td>HsubM = (CInt (HsubM * 100 * Fact1)) / 100 '(CInt (HsubM * Fact1 * 10)) / 100 <(Version 1 for C5D Perthometer)</td>
<td></td><td></td><td> 2365</td><td>HsubS - (CInt (HsubS * 100 * Fact1)) / 100 '(CInt (HsubS * Fact1 * 10)) / 100 <(Version 1 for C5D Perthometer)</td>
<td></td><td> 10</td><td> 2370</td><td>Rem Convert P from Points to Millimeters</td>
<td> 15</td><td></td><td> 2375</td><td>PsubM = (CInt (PsubM * Fact3 * 100)) / 100</td>
<td></td><td></td><td> 2380</td><td>PsubS = (CInt (PsubS * Fact3 * 100)) / 100</td>
<td></td><td></td><td></td><td>'SetValues for SaveData SubRoutine</td>
<td></td><td> 15</td><td></td><td>PsubMsave (i) = PsubM PsubSsave (i) = PsubS</td>
<td> 20</td><td></td><td> 2560</td><td>HsubMsave (i) = HsubM HsubSsave (i) = HsubS NPsave (i) = NP 20 RIPm = RIPm + PsubM</td>
<td></td><td></td><td> 2565</td><td>RlHm = RIHm + HsubM</td>
<td> 25</td><td></td><td> 2570</td><td>Next and</td>
<td></td><td></td><td> 2575</td><td>RIPm = (CInt (RlPm * 100 / NTraces)) / 100</td>
<td></td><td> 25</td><td> 2580</td><td>RIHm = (CInt (RIHm * 100 / NTraces)) / 100</td>
<td></td><td></td><td> 2585</td><td>WvIdx = RlPm * RlHm</td>
<td></td><td></td><td></td><td>DoEvents</td>
<td> 30</td><td> 30</td><td colspan="2">End Sub</td>
EP 1 874 535 B1
Contents7
38 members in 21 offices
Priority claims8
| Document | Office | Kind | Date |
|---|---|---|---|
| 6177805 | United States of America | A | |
| 6177805 | United States of America | A | |
| 06735846 | European Patent Office (EPO) | A | |
| 2006006357 | United States of America | W | |
| 2006006357 | United States of America | W | |
| EP20060735846 | – | – | – |
| US20050061778 | – | – | – |
| WO2006US06357 | – | – | – |
Members38
| Document | Office | Kind | |
|---|---|---|---|
| US2006188695A1 | United States of America | A1 | |
| AU2006216656A1 | Australia | A1 | |
| CA2597735A1 | Canada | A1 | |
| WO2006091707A1 | World Intellectual Property Organization (WIPO) | A1 | |
| MX2007009813A | Mexico | A | |
| NO20074685L | Norway | L | |
| KR20070104600A | Republic of Korea | A | |
| EP1874535A1 | European Patent Office (EPO) | A1 | |
| CN101119843A | China | A | |
| IL185254A0 | Israel | A0 | |
| IL185254D0 | Israel | D0 | |
| EP1874535B1 | European Patent Office (EPO) | B1 | |
| AT400429T | Austria | T | |
| ATE400429T1 | Austria | T1 | |
| PT1874535E | Portugal | E | |
| JP2008531770A | Japan | A | |
| DE602006001746D1 | Germany | D1 | |
| DK1874535T3 | Denmark | T3 | |
| ES2307285T3 | Spain | T3 | |
| PL1874535T3This record | Poland | T3 | |
| RU2007134242A | Russian Federation | A | |
| BRPI0607853A2 | Brazil | A2 | |
| UA90705C2 | Ukraine | C2 | |
| RU2404894C2 | Russian Federation | C2 | |
| NZ561552A | New Zealand | A | |
| AU2006216656B2 | Australia | B2 | |
| CN101119843B | China | B | |
| JP5025494B2 | Japan | B2 | |
| KR101216918B1 | Republic of Korea | B1 | |
| US8551600B2 | United States of America | B2 | |
| US2013273318A1 | United States of America | A1 | |
| US2014000789A1 | United States of America | A1 | |
| IL185254A | Israel | A | |
| US9096037B2 | United States of America | B2 | |
| US9096038B2 | United States of America | B2 | |
| US2015298447A1 | United States of America | A1 | |
| US9452598B2 | United States of America | B2 | |
| BRPI0607853B1 | Brazil | B1 |
Numbers
- Publication, DOCDB
- 1874535
- Publication, EPODOC
- PL1874535T
- Application
- 735846
- Application, DOCDB
- 06735846
- Application, EPODOC
- PL20060735846T
Titles2
- English
- LOW DISTORTION INTERLAYER
- Polish
- Warstwa pośrednia o niskim zniekształceniu
Classification
- CPC, 23
- B29D7/01
- B32B17/10036
- B32B37/24
- B29C59/005
- B29K2029/00
- B32B17/10339
- B32B17/10577
- B32B17/10761
- Y10T156/10
- Y10T156/1039
- Y10T428/24355
- B32B17/10449
- B32B17/10587
- B32B17/10889
- B32B17/10935
- D06N7/00
- B29C59/04
- B32B37/182
- B32B2367/00
- B29L2007/002
- B32B2307/42
- B32B2457/20
- B32B2551/00
- IPC, 3
- B32B17 10
- B29C59 00
- B29D7 01