US20040202800A1 - Solid surface products - Google Patents

Solid surface products Download PDF

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Publication number
US20040202800A1
US20040202800A1 US10762206 US76220604A US2004202800A1 US 20040202800 A1 US20040202800 A1 US 20040202800A1 US 10762206 US10762206 US 10762206 US 76220604 A US76220604 A US 76220604A US 2004202800 A1 US2004202800 A1 US 2004202800A1
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Prior art keywords
matrix
solid surface
surface structure
made
flat non
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Abandoned
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US10762206
Inventor
Dennis Schober
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Lumicor Inc
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Schober Inc
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/14Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
    • B32B37/16Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with all layers existing as coherent layers before laminating
    • B32B37/18Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with all layers existing as coherent layers before laminating involving the assembly of discrete sheets or panels only
    • B32B37/182Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with all layers existing as coherent layers before laminating involving the assembly of discrete sheets or panels only one or more of the layers being plastic
    • B32B37/185Laminating sheets, panels or inserts between two discrete plastic layers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00Layered products comprising a layer of synthetic resin
    • B32B27/06Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B27/08Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00Layered products comprising a layer of synthetic resin
    • B32B27/12Layered products comprising a layer of synthetic resin next to a fibrous or filamentary layer
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B3/00Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar form ; Layered products having particular features of form
    • B32B3/02Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar form ; Layered products having particular features of form characterised by features of form at particular places, e.g. in edge regions
    • B32B3/08Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar form ; Layered products having particular features of form characterised by features of form at particular places, e.g. in edge regions characterised by added members at particular parts
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/0007Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding involving treatment or provisions in order to avoid deformation or air inclusion, e.g. to improve surface quality
    • B32B37/003Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding involving treatment or provisions in order to avoid deformation or air inclusion, e.g. to improve surface quality to avoid air inclusion
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B44DECORATIVE ARTS
    • B44CPRODUCING DECORATIVE EFFECTS; MOSAICS; TARSIA WORK; PAPERHANGING
    • B44C5/00Processes for producing special ornamental bodies
    • B44C5/005Processes for producing special ornamental bodies comprising inserts
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B44DECORATIVE ARTS
    • B44CPRODUCING DECORATIVE EFFECTS; MOSAICS; TARSIA WORK; PAPERHANGING
    • B44C5/00Processes for producing special ornamental bodies
    • B44C5/04Ornamental plaques, e.g. decorative panels, decorative veneers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B44DECORATIVE ARTS
    • B44FSPECIAL DESIGNS OR PICTURES
    • B44F1/00Designs or pictures characterised by special or unusual light effects
    • B44F1/06Designs or pictures characterised by special or unusual light effects produced by transmitted light, e.g. transparencies, imitations of glass paintings
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2327/00Polyvinylhalogenides
    • B32B2327/06PVC, i.e. polyvinylchloride
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2333/00Polymers of unsaturated acids or derivatives thereof
    • B32B2333/04Polymers of esters
    • B32B2333/12Polymers of methacrylic acid esters, e.g. PMMA, i.e. polymethylmethacrylate
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2369/00Polycarbonates
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2451/00Decorative or ornamental articles

Abstract

A flat non-porous unitary solid surface product comprised of: (a) a flat non-porous unitary matrix made of polymethylmethacrylate, polyvinyl chloride, polycarbonate, or combinations thereof; and (b) a visible decorative object that is permanently fixated in the matrix, wherein the decorative object extends to least one edge of the matrix. A method for manufacturing the flat non-porous unitary solid surface product.

Description

    CROSS-REFERENCE TO RELATED APPLICATION
  • This application claims the benefit of U.S. Provisional Application No. 60/307,898 filed Jul. 25, 2001.[0001]
  • FIELD OF THE INVENTION
  • The present invention relates to flat non-porous unitary solid surface structures, and more particularly, to flat non-porous unitary solid surface products comprised of: (1) a matrix made of polymethylmethacrylate, polyvinyl chloride, polycarbonate, or combinations thereof; and (2) one or more visible decorative objects that are permanently fixated in the matrix, and methods for manufacturing these products. These manufacturing methods do not involve using a mold or casting a liquid resin around the decorative object to be fixated. The solid surface products of the invention provide strikingly beautiful and unusual visual effects that are difficult to describe in words. [0002]
  • BACKGROUND OF THE INVENTION
  • Solid surface products made of cured polymethylmethacrylate containing fine microscopic particles of inert inorganic fillers are known in the art. It is believed that all of the prior art polymethylmethacrylate solid surface products are made by using a mold and by casting therein a liquid acrylic resin which is then cured to form polymethylmethacrylate. For example, E. I. DuPont de Nemours and Company originated the solid surface category of products more than thirty years ago when it introduced the synthetic product sold under the trademark CORIAN which is believed to be a polymethylmethacrylate matrix containing large amounts of microscopic particles of inert inorganic fillers. It is believed that CORIAN is made by casting a liquid acrylic resin in a mold of some type and then curing the resin to form polymethylmethacrylate. CORIAN is usually an opaque product which mimics the decorative effect of marble. CORIAN is useful for kitchen countertops, kitchen sinks, bathroom lavatories, desktops, windowsills, and the like. Several patents owned by DuPont describe casting plastic simulated marble building products which are believed to be CORIAN. See Slocum U.S. Reissue Pat. No. Re 27,093, Duggins U.S. Pat. No. 3,488,246, Duggins et al. U.S. Pat. No. 3,6342,975, Duggins U.S. Pat. No. 3,847,865, and Duggins et al. U.S. Pat. No. 4,107,135. In general terms, these DuPont patents describe cast products which are made of cured polymethylmethacrylate containing 30% to 80% by weight of microscopic particles (for example, particles having an average size of 7 microns) of inert inorganic fillers such as calcium carbonate, calcium sulfate, clay, silica, glass, calcium silicate, alumina, carbon black, titania, powdered metals, and alumina trihydrate. [0003]
  • Other synthetic solid surface products are sold by Avonite, Inc. under the trademark AVONITE which mimic the decorative effect of artificial stone. Risley U.S. Pat. No. 5,286,290 assigned to Avonite, Inc. describes dehydrating alumina trihydrate, rehydrating with a solution of dye, drying the solution to make colored alumina trihydrate, adding the colored alumina trihydrate to a resin matrix containing inert fillers, and cast to make a fire retardant solid decorative material having the appearance of artificial granite. The resin matrix may be ortho or iso polyesters, acrylics, or polycarbonates. The product may be in the form of a sheet or slab for kitchen countertops and decorative architectural surfaces or facades. [0004]
  • Eckart et al. U.S. Pat. No. 5,958,539 assigned to Eastman Chemical Company discloses a thermoplastic article having a fabric comprised of textile fibers embedded therein produced by applying heat and pressure to a laminate comprising, in order, (1) an upper sheet material, (2) a fabric comprised of textile fibers, and (3) a lower sheet material to produce a thermoplastic article having the fabric embedded therein. The upper and lower sheet materials are specifically made of a PETG copolyester available from Eastman Chemical Company. PETG is the acronym for polyethylene terephthalate glycol. [0005]
  • A similar patent is Eckart et al. U.S. Pat. No. 5,998,028 assigned to Eastman Chemical Company which discloses a thermoplastic article having metallic wire, rod, and/or bar embedded therein produced by applying heat and pressure to a laminate comprising, in order, (1) an upper sheet material, (2) metallic wire, rods, or bars, and (3) a lower sheet material to produce a thermoplastic article having the metallic wire, rod, and/or bar embedded therein. As in Eckart et al. U.S. Pat. No. 5,958,539 above, the upper and lower sheet materials are specifically made of a PETG copolyester available from Eastman Chemical Company. [0006]
  • Another similar patent is Eckart et al. U.S. Pat. No. 6,025,069 assigned to Eastman Chemical Company which discloses a thermoplastic article having a high-relief, molded or embossed surface produced by contacting a laminate comprising a first or outer copolyester sheet material and a second or backing copolyester sheet material with heat and pressure using a heated element which simultaneously causes the material to be bonded and a high-relief, decorative appearance to be produced on at least one surface of the thermoplastic article. Also disclosed is an embossed or molded, bonded laminate comprising, in order, (1) a first or outer copolyester layer, (2) a second layer comprising a film which is colored or which bears an image or pattern, and (3) a third or backing copolyester layer, wherein the first and third layers are composed on the copolyester. As in Eckart et al. U.S. Pat. No. 5,958,539 and Eckart et al. U.S. Pat. No. 5,998,028 above, the copolyester layers are specifically made of a PETG copolyester available from Eastman Chemical Company. [0007]
  • Prior to the present invention, there existed a long-felt need for a dry process for making a unitary solid surface product comprised of: (I) a matrix made of polymethylmethacrylate, polyvinyl chloride, polycarbonate, or combinations thereof; and (2) one or more visible decorative objects (objects that are visible to the unaided human eye) that are permanently fixated in the matrix. It was believed by knowledgeable people in the plastics industry that it was not possible to make such a solid surface product without using a mold and casting therein a liquid resin around the object to be fixated. It is believed that researchers who attempted to make such products using a dry process (that is, without using a mold and casting a liquid resin around the object to be fixated) produced products which contained defects such as air bubbles entrapped in the matrix, voids in the matrix, or cracks in the matrix. [0008]
  • Extensive research finally led to the present invention which allows an object to be fixated in a unitary matrix made of polymethylmethacrylate, polyvinyl chloride, polycarbonate, or combinations thereof, without using a mold and casting therein a liquid resin around the object. In addition, the present invention provides aesthetically-pleasing products which are free of defects of the type referred to above. [0009]
  • SUMMARY OF THE INVENTION
  • In one embodiment the invention is a flat non-porous unitary solid surface structure comprised of: (a) a flat non-porous unitary thermoplastic polymeric matrix made of polymethylmethacrylate, polyvinyl chloride, polycarbonate, or combinations thereof; and (b) a visible decorative object that is permanently fixated in the matrix, wherein the decorative object extends to least one edge of the matrix. [0010]
  • In another aspect the invention is a method for manufacturing the flat non-porous unitary solid surface structure including the steps of: (a) providing a first flat non-porous unitary thermoplastic polymeric sheet made of polymethylmethacrylate, polyvinyl chloride, or polycarbonate; (b) placing a decorative object on the first sheet of polymeric material wherein the decorative object extends beyond at least one edge of the first sheet of polymeric material; (c) placing a second flat non-porous unitary thermoplastic polymeric sheet of made of polymethylmethacrylate, polyvinyl chloride, or polycarbonate on top of the decorative object wherein the decorative object also extends beyond at least the corresponding edge of the second sheet of polymeric material, whereby a lay-up sandwich is formed comprised of the first flat sheet of polymeric material, the decorative object which extends beyond at least one edge of both of the sheets of polymeric material, and the second flat sheet of polymeric material; (d) loading the lay-up sandwich into a press; (e) applying a predetermined amount of heat and pressure to the lay-up sandwich for a predetermined period of time; (f) opening the press to allow air and gases to escape from the lay-up sandwich; (g) closing the press and applying a predetermined amount of heat and pressure to the lay-up sandwich for a predetermined period of time whereby the first and second polymeric material sheets melt together in the lay-up sandwich to provide a unitary product; and, (h) allowing the product to cool while maintaining the pressure at a predetermined level until the product reaches a predetermined temperature at which point the press is opened and the product is removed from the press.[0011]
  • BRIEF DESCRIPTION OF THE DRAWINGS
  • FIG. 1 is a pictorial or three-dimensional view of one embodiment of the invention illustrating a unitary solid surface product having a matrix made of polymethylmethacrylate, polyvinyl chloride, polycarbonate, or combinations thereof, and decorative objects that are permanently fixated in the matrix. In this example, the fixated objects consist of dried long-stem grass. [0012]
  • FIG. 2 is an exploded pictorial view illustrating the starting materials employed in making the product shown in FIG. 1. In this example, the starting materials are an upper sheet made of polymethylmethacrylate, polyvinyl chloride, or polycarbonate material, the objects to be fixated consist of dried long-stem grass, and a lower sheet made of polymethylmethacrylate, polyvinyl chloride, or polycarbonate material. [0013]
  • FIG. 3 is a pictorial view illustrating the product shown in FIG. 1 in a finished stage of production before trimming. [0014]
  • FIG. 4 is an exploded pictorial view illustrating the starting materials employed in making a second embodiment of the invention. In this example, the starting materials are an upper sheet of polymethylmethacrylate, polyvinyl chloride, or polycarbonate material, an intermediate sheet of polymethylmethacrylate, polyvinyl chloride, or polycarbonate material that has been textured on both surfaces, and a lower sheet of polymethylmethacrylate, polyvinyl chloride, or polycarbonate material. [0015]
  • FIG. 5 is a vertical cross-sectional view of the product of FIG. 1 when viewed in the direction of the arrows [0016] 5-5 in FIG. 1. The phantom line in FIG. 5 indicates the location where the inner surfaces of two sheets of polymeric material interfaced before they melted together in the manufacturing process.
  • DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
  • The present invention provides non-porous unitary solid surface products and methods for manufacturing the same. By the tern “unitary,” it is meant that the products are physically an undivided single piece, and therefore they are not a laminate structure consisting of separate layers that can be separated or delaminated. It should be understood that some products of the invention might visually appear (to the unaided human eye) to be a laminate of separate layers which maintain their integrity, but this visual appearance is not correct. The layers of polymeric starting material have in fact melted together and have become an undivided single piece. From the standpoint of aesthetically-pleasing visual appearance, line drawings and words are not capable of describing the strikingly beautiful and unusual visual effects provided by the solid surface products of the invention. The inventive solid surface products may be employed to make countertops, sinks, lavatories, desktops, table tops, chairs, windowsill, and the like. [0017]
  • The first embodiment of the invention, illustrated by the product in FIG. 1, is a flat non-porous unitary polymeric solid surface structure [0018] 10 comprised of a matrix 12 made of clear polymethylmethacrylate, polyvinyl chloride, polycarbonate, or combinations thereof, and one or more visible decorative objects 14 (that is, objects that are visible to the unaided human eye) that are permanently fixated in the matrix 12. In the example illustrated by FIG. 1, the fixated decorative objects 14 consist of dried long-stem grass. As shown in FIG. 1, the fixated decorative objects 14 appear to float in the transparent matrix 12. The outer surfaces of the solid surface structure may have any desired finish, such matte, semi-gloss, or high gloss. The flat structure 10 may be subjected to conventional thermoforming/shaping processes if a non-flat shape is desired.
  • FIG. 5 is a vertical cross-sectional view of product [0019] 10 viewed in the direction of the arrows 5-5 shown in FIG. 1. The phantom line 20 in FIG. 5 indicates the location where the inner surfaces of polymeric sheets 16 and 18 interfaced before they melted together in the manufacturing process (as will be described below).
  • The Basic Lay-Up Sandwich
  • The unitary solid surface structures [0020] 10 constructed according to the first embodiment of the present invention contain fixated decorative objects 14. The decorative objects 14 can be made of various materials as will be described below. FIG. 2 illustrates how a solid surface structure of this invention is made from a basic lay-up sandwich consisting of the following starting materials: (1) a bottom sheet 16 made of polymethylmethacrylate, polyvinyl chloride, or polycarbonate material; (2) one or more layers of a decorative material 14 (the object to be fixated) which also functions as a breather layer for air and gases to escape during the manufacturing process; and, (3) a top sheet made of polymethylmethacrylate, polyvinyl chloride, or polycarbonate material. As shown in FIG. 2, during lay up the decorative material 14 extends beyond the edges of polymeric sheets 16 and 18. As mentioned above, decorative material 14 provides an escape path for air, water vapor, and gases generated during the pressing operation. Prior to the pressing operation, the decorative material 14 that extends beyond the edges of polymeric sheets 16 and 18 is pulled taunt and taped to a caul plate (as will be described below).
  • Variations on this basic lay-up sandwich may include more than two layers of polymeric sheet and multiple layers of decorative materials, alternating one and then the other. For example, the basic lay-tip sandwich may consist of: (1) a top sheet of polymeric material; (2) a first layer of decorative material; (3) an intermediate sheet of polymeric material; (4) a second layer of a decorative material; and, (5) a bottom sheet of polymeric material. [0021]
  • The thickness of product [0022] 10 may range from about 0.030 inch (0.7937 mm) to 2.0 inches (50.80 mm). However, thicker and thinner gauges are possible based on the press capabilities and starting material availability.
  • Polymethylmethacrylate, Polyvinyl Chloride, and Polycarbonate Starting Materials
  • The non-porous polymeric sheets [0023] 16 and 18 may be clear (transparent), colored, textured (on one or both faces), frosted, translucent, opaque, and they may also contain fire-retardant additives and performance additives.
  • The polymeric sheets [0024] 16 and 18 may vary in thickness from about 0.004 inch (0.100 mm) to 1.0 inch (25.4 mm). Also, the polymeric sheets 16 and 18 in the basic lay-up sandwich may vary in thickness from each other.
  • Polymethylmethacrylate sheet material can be manufactured casting or by extrusion. The preferred polymethylmethacrylate sheet material is made by extrusion and has more consistent gauge. Polymethylmethacrylate sheet material made by casting has inconsistent gauge (hills and valleys) which will cause problems with air and gas entrapment and also gloss/texture problems on the surface of the product caused by pressure variations. [0025]
  • The preferred polymethylmethacrylate sheet material has the following properties: [0026]
    ASTM Test
    Method Units Value
    Physical Properties
    Specific Gravity D-792 1.19
    Optical Refractive D-542 1.49
    Index
    Light Transmittance D-1003
    Index
    (sample thickness
    0.100 inch)
    Total % 92
    Haze % 2
    Sound Transmission E90-70 27
    (0.125 inch Thickness) E 413
    Water Absorption D-570 % 0.4
    by weight
    Shrinkage D-702 % <5%
    shrinkage
    Mechanical Properties
    Tensile Strength, D-638 psi 10,100
    Maximum
    Tensile Elongation, % 5.1
    Maximum
    Modulus of Elasticity psi 431,000
    Flexural Strength, D-790 psi 14,600
    Maximum
    Izod Molded Notch D-256-56 Ft lbs/inch 0.4
    ½ inch × 2½ inch ×
    ¼ inch of notch
    bar
    at 73° F.
    Izod Milled Notch Ft lbs/inch 0.28
    ½ inch × 2½ inch ×
    ¼ inch of notch
    bar
    at 73° F.
    Tensile Impact D-1822 Ft lbs/in2 20
    Strength
    Abrasion Resistance D-1044
    0 cycles Haze % 2
    10 cycles Haze % 15
    50 cycles Haze % 30
    200 cycles Haze % 50
    Rockwell Hardness D-785 M-93
    (sample thickness
    0.25 inch)
    Thermal Properties
    Maximum ° F. 170-190
    Recommended
    Continuous Service
    Temperature
    Softening ° F. 210-220
    Temperature
    Melting ° F. 300-315
    Temperature
    Deflection D-648
    Temperature
    Load, Unannealed
    3.6° F./minute, ° F. 190
    264 psi
    3.6° F./minute, ° F. 205
    66 psi
    Coefficient of Thermal D-696 Ins/in/° F. × 10°
    Expansion
     −40° F. 2.7
     −20° F. 2.9
       0° F. 3.1
       20° F. 3.2
       40° F. 3.4
       60° F. 3.6
       80° F. 3.9
      100° F. 4.3
    Thermal Conductivity C-177 BTU 0.9
    (Hr) (Ft2) (° F./in)
    Flammability D-635 Ins/minute
    (Burning Rate) 0.060 inch 1.019
    0.236 inch 0.318
    Smoke Density Rating D-2843-77 %
    0.236 inch 0.36
    Self-Ignition Temp D-1929 ° F. 833
    0.236 inch
    Flame Spread Index/ 0.375 inch 110
    Smoke Developed E-84-86 0.236 inch 115
    Index
    Chemical Properties
    Resistance to Stress- ARTC
    Critical Crazing modification
    stress to: of
    MIL-P-6997
    Isopropyl Alcohol psi 900
    Lacquer Thinner psi 500
    Toluene psi 1,300
    Solvesso 100 psi 1,600
  • The preferred polyvinyl chloride sheet material has the following properties and is sold under the trademark INTEDUR TYPE II by World-Pak Corporation/Inteplast Corporation, Livingston. N.J.: [0027]
    Properties Test Method Units Value
    PHYSICAL
    Thickness ASTM D1505 in. {fraction (1/16)} inch˜
    ½ inch
    Density ASTM D792 g/cm3 1.33˜1.41
    MECHANICAL
    Tensile Strength @ ASTM D638 psi 6,000˜8,000
    Yield
    Elongation @ ASTM D638 % 30˜70
    Break
    Flexural Modulus ASTM D790 psi 300,000-400,000
    Flexural Strength @ ASTM D790 psi  6,000˜10,000
    Yield
    Izod Impact ASTM D256 ft-lbs./in.  5˜17
    Strength (Notched)
    Shore Hardness ASTM D2240 D 73˜81
    (D scale)
    THERMAL
    Heat Deflection ASTM D648 ° F. 145-155
    Temperature
    Vertical Burn Test UL 94 V-O
  • The preferred polycarbonate sheet material has the following properties and is sold under the trademark LEXAN 9600 by General Electric Company, Pittsfield, Mass.: [0028]
    Property Test Method Units Value
    PHYSICAL
    Specific Gravity ASTM D792 1.25
    Water Absorption, ASTM D570 % 0.20
    Equilibrium, 24 Hrs
    Light Transmission ASTM D1003 % 85
    (avg.), 0.125 inch
    thickness
    MECHANICAL
    Tensile Strength ASTM D638 psi
    @ Yield 9,500
    Ultimate 9,000
    Elongation ASTM D638 % 95
    Tensile Modulus ASTM D638 psi 235,000
    Flexural Strength ASTM D790 psi 13,500
    Flexural Modulus ASTM D790 psi 370,000
    Compressive Strength ASTM D695 psi 12,500
    Dynatup Impact ASTM D3783 ft-lbs 50
    Strength,
    ½ inch dia.
    dart, (gauge
    dependant), @
    73° F.
    Gardner Impact Strength, ASTM D3029 in-lbs. >320
    round tup
    (gauge dependant), @
    73° F.
    Izod Impact Strength ASTM D256A ft-lbs./
    (gauge dependant) in.
    Notched @ 73° F. 2.4
    Unnotched @ 73° F. NB
    THERMAL
    Coefficient of Thermal ASTM D696 in./in./ 3.75 × 10−5
    Expansion ° F.
    Heat Deflection ASTM D648 ° F. 280
    Temperature
    @ 264 psi
    FLAMMABILITY
    UL Flammability UL 94 V-0 (90
    mils and
    above)
    V-2
    (34-89 mils)
    FAA Flammability @ FAR 25.853 Passes
    40 to 125 mils A & B
    ATS 1000 @ Pass
    40 to 125 mils
  • Materials for Decorative Object to be Fixated
  • The material [0029] 14 to be fixated in the polymeric matrix 12 may be made of textile fabric, paper, plastic film, plastic sheet, metallic wire, rod, mesh, bar, wood veneer, and various dried natural materials (such as the long-stem grass illustrated in FIG. 1), tree bark, plant leaves, petals, and twigs). It is important that the material be dry to avoid giving off water vapor or steam during the manufacturing process.
  • The material [0030] 14 may be one or more layers of a textile fabric made of various fibers. Textile fabrics can impart beautiful and unusual visual effects to the product, such as an iridescent effect or a moiré effect. Non-limiting examples of suitable textile fabrics are: synthetic, semi-synthetic, naturally occurring and polymeric, including for example, rayon, polyester, nylon, synthetic polyamides (such as nylon 66 and nylon 6), acrylic, modacrylic, cellulose acetate, cotton, wool, silk and fiberglass. The fabric may be woven, knitted, spun-bonded, or prepared by other well-known processes in the textile trade. The fabric may be printed, coated, dyed, sublimated or decorated by other techniques known within the textile trade. Fabrics with loose weaves and have as open area of 0.005 inch or greater between yarns/threads are best. Fabrics with rough and porous surfaces are also preferred over smooth surfaces. Tightly woven fabrics with smooth surfaces will not function in the thermal melting process because they prevent resin transfer through the material. Natural fibers are preferred due to their porosity. The melted resin saturates such fibers more readily. The textile fabric may vary in thickness from about 0.00045 inch (0.0114 mm) to 0.25 inch (6.35 mm).
  • As mentioned above, the material [0031] 14 to be fixated in the matrix 12 may also be made of wood veneer, paper, dried plant fibers and parts. Non-limiting examples are: cellulose, cotton, linen, pulp, rag, dried plant materials and fibers including long-stem grass, leaves, petals, bark and twigs from reed, bamboo, papyrus, banana, mulberry, and wicker. For these types of material, the thickness of the layer may be from about 0.00045 inch (0.0114 mm) to 0.25 inch (6.35 mm).
  • The material [0032] 14 to be fixated in the polymeric matrix 12 may also be made of dry metal. Non-limiting examples are: copper, bronze, brass, steel, stainless steel, iron, nickel, and aluminum. Variety of shapes including: rod, mesh, sheet, perforated sheet, foil, strips, shavings, woven, and cable. The metal may be decorated such as etched, anodized, sanded, brushed, stained, painted, printed, chemically treated, galvanized, corroded, aged, polished, and plated. For these types of material, the thickness of the layer may be from about 0.00045 inch (0.0114 mm) to 1.0 inch (25.4 mm).
  • The material [0033] 14 to be fixated in the matrix 12 may also be a plastic sheet or film. Non-limiting examples are: polymethylmethacrylate, polycarbonate, polyvinyl chloride, PETG copolyester, polyethylene, polypropylene, polyester, polyvinylidinefluoride (PVDF) (sold under the trademark KYNAR), polyvinylfluoride (PVF) (sold under the trademark TEDLAR), and polyurethane. For these types of material, the thickness of the layer may be from about 0.00045 inch (0.0114 mm) to 1.0 inch (25.4 mm).
  • Manufacturing Processes
  • The invention also includes methods for manufacturing the unitary solid surface structure [0034] 10. These manufacturing methods do not involve using a mold and casting a liquid resin around the object to be fixated.
  • In order to produce products [0035] 10 which are free of defects (such as air or gas bubbles entrapped in the matrix, voids in the matrix, or cracks in the matrix), it has been found to be critical to process the above-described basic lay-up sandwich according to the following operating parameters. These process parameters work well with most paper and fabric decorative materials.
  • First, the basic lay-up sandwich must be processed in a heated press that can apply the required heat and pressure to melt the polymeric sheets [0036] 16 and 18 together and thereby create the matrix 12 that fixates the one or more decorative objects 14 within the matrix. Most preferred is a steam heated multiple opening press.
  • Second, when using the preferred polymeric sheets described above, the press should be preheated to a temperature of about 280° F. Then the lay-up sandwich is loaded into the press. The press is then closed against the lay-up sandwich at a pressure of about 40 pounds per square inch (psi). The press temperature is then ramped up until the lay-up sandwich reaches a temperature of about 290° F.-310° F. while maintaining the pressure at about 40 psi. This temperature works well for polymethylmethacrylate and polyvinyl chloride. Polycarbonate requires a higher temperature of about 350° F.-375° F. [0037]
  • Third, at this point the press must be opened and all pressure is removed from the lay-up sandwich. This step is referred to as “bumping” the press. This step is critical in order to allow the heated air, water vapor, and gases to escape from between the polymeric sheets [0038] 16 and 18 in the lay-up sandwich so that bubbles or voids are not entrapped in the matrix 12.
  • Fourth, the press is then closed against the lay-up sandwich and the pressure is ramped up to about 160 psi. The press temperature is then ramped up until the materials in the lay-up sandwich reach about 290° F.-310° F. while maintaining the pressure at about 160 psi. Again, this temperature works well for polymethylmethacrylate and polyvinyl chloride, but polycarbonate requires a higher temperature of 350° F.-375° F. This pressure and temperature is then held for about 1 to 6 minutes depending on the thickness of the lay-up sandwich to allow the polymeric sheets [0039] 16 and 18 to melt together in the lay-up sandwich.
  • Fifth, the heat is turned off and the product is allowed to gradually cool while maintaining the pressure at about 160 psi until the product reaches a temperature of about 100° F. at which point the press is opened and the product (which needs some trimming) is removed from the press. If needed, a coolant may be circulated through the platens to cool the press. This step of gradually cooling the product is important because the product is being annealed, thereby removing the internal strains resulting from the previous operations. This prevents the polymeric matrix [0040] 12 from developing cracks, warping, or excessive shrinking.
  • Prior to full-scale production, the compatibility between specific decorative materials and the polymeric sheets should be evaluated. Some decorative materials can degrade under heat and pressure resulting in discoloration, color bleed, and separation. [0041]
  • During the pressing process, the outer surface of the polymeric sheets can optionally be deeply embossed or also textured using coated release papers or release films. A variety of suitable textured release papers are available from the S. D. Warren Company, Westbrook, Me. A variety of release films are available from the DuPont Company, Wilmington, Del. The release papers and release films have specific textures and gloss levels that are transferred onto the polymeric sheets during the pressing/heating, operation. The release papers and release films also separate the polymeric sheets from the caul plate (described in Example 1 below) and thereby they prevent the polymeric sheets from sticking to the caul plate. [0042]
  • Refinishing
  • One of the advantages of the solid surface structures of the invention is that if they become scratched or marred, they are capable of being restored and refinished. The is particularly important for applications such as table tops and countertops. Refinishing may be accomplished for matte, semi-gloss, and high gloss finishes. The preferred process for refinishing uses an orbital disc sanding machine and film abrasives sold under the trademark TRIZACT and disc sanding pads sold under the trademark HOOKIT II, both products of Minnesota Mining and Manufacturing Co., St. Paul, Minn. The process involves sanding out the defects in the surface and then polishing. [0043]
  • Optional Features
  • During the pressing/heating operation, specialty films can also be applied one or both of the polymeric sheets to enhance the abrasion resistance, chemical resistance, and ultraviolet resistance of the final product. These specialty films may be made of various materials including polyester, polyvinylfluoride (PV F), ethylene trifluoroethylene (ETFE), fluorinated ethylenepropylene (FEP), polyvilylidenefluoride (PVDF), and chlorotrifluoroethylene (CTFE). [0044]
  • These specialty films can be on the top and/or bottom of the final product. Typically, these films have a higher melt point than polymethylmethacrylate and therefore require the use of a heat-activated adhesive coating, which is applied to the film prior to the pressing/heating operation. Generally, the specialty film has a thickness of 0.004 inch (0.100 mm) to 0.020 inch (0.500 mm). [0045]
  • EXAMPLE 1
  • In this example, the basic lay-up sandwich consists of three layers of the following starting materials: (1) a bottom sheet of the preferred polymethylmethacrylate material that is 0.060 inch thick, 48 inches wide, and 96 inches long; (2) a decorative textile fabric that is 58 inches wide and 102 inches long; and (3) a top sheet of the preferred polymethylmethacrylate that is 0.060 inch thick, 48 inches wide, and 96 inches long. [0046]
  • The final lay-up book is made as follows. A textured sheet of release paper that is 60 inches wide and 100 inches long is placed on a 0.060 inch thick aluminum caul plate and taped to the caul plate. The basic lay-up sandwich (described in the paragraph above) is placed on top of the textured sheet of release paper. The textured sheet of release paper will impart an aesthetically-pleasing texture to the outer surface of the bottom sheet of polymethylmethacrylate. The decorative textile fabric extending beyond the edges of polymethylmethacrylate sheets is pulled taunt and taped to the caul plate. Another sheet of textured release paper that is 60 inches wide and 100 inches long is placed on top of the basic lay-up sandwich. This textured sheet of release paper will impart an aesthetically-pleasing texture to the outer surface of the top sheet of polymethylmethacrylate. Another caul plate is placed on top of the upper sheet of textured release paper and the upper textured sheet of release paper is taped to the caul plate. Thermocouples are attached to the lay-up sandwich so that the temperature of the sandwich can be accurately measured. [0047]
  • Four plies of canvas are placed below the bottom caul plate and above the top caul plate to event) distribute the pressure and heat during the pressing/heating operation. The book is placed on a (0.125 inch thick aluminum sheet loader pan to facilitate loading and unloading of the book into the press. [0048]
  • The press is preheated to a temperature of about 280° F. Then the final lay-up book is loaded into the press. The press is closed against the book at a pressure of about 40 psi. The press temperature is then ramped up until the lay-up sandwich reaches a temperature of about 290° F.-310° F. while maintaining the pressure at about 40 psi. The press is opened and all pressure is removed from the book. The press is closed against the book and the pressure is ramped up to about 160 psi. The press temperature is ramped up until the materials in the lay-up sandwich reach a temperature of about 290° F.-310° F. while maintaining the pressure at about 160 psi. This pressure and temperature is then held for about 1 to 6 minutes depending on the thickness of the lay-up sandwich to allow the polymethylmethacrylate sheets to melt together in the lay-up sandwich to provide a unitary product. [0049]
  • The heat is then turned off and the product is allowed to gradually cool while maintaining the pressure at about 160 psi until the product reaches a temperature of about 100° F. at which point the press is opened and the product (which may need some trimming) is removed from the press. [0050]
  • Example 1 can also be performed using polyvinyl chloride or polycarbonate, but polycarbonate requires the higher temperature of 350° F.-375° F. Example 1 can also be performed using a combination of polymethylmethacrylate, polyvinyl chloride, or polycarbonate. There are benefits in combining the properties of two thermoplastics. For example, by combining polyvinyl chloride and polymethylmethacrylate, the polyvinyl chloride will improve the flammability and chemical resistance of the polymethylmethacrylate, and the polymethylmethacrylate will improve the clarity, ultra-violet resistance, and abrasion resistance of the polyvinyl chloride. The thermoplastics need to be formulated to have similar processing temperatures to work in the press process. [0051]
  • EXAMPLE 2
  • In this example, the thickness of the product is 0.25 inch or greater. When fabricating products in a thickness of 0.25 inch or greater employing delicate decorative papers, fabrics, or organic materials, a first stage is necessary to encapsulate the decorative material within two thin sheets of 0.060 inch polymethylmethacrylate to prevent tearing of the decorative material caused by movement of the polymethylmethacrylate during pressing. The thinner sheets of polymethylmethacrylate will hold the decorative material in place with minimal movement during stage two. The two-stage process enables products to be made in thicker gauges with less “melt out.” Thus, maximum thickness is preserved. The goal is to transfer heat to the lay-up sandwich to melt the polymethylmethacrylate sheets together using the least amount of heat, pressure, and time. [0052]
  • In stage 1, a 0.12 inch intermediate product with 0.005 inch relief texture is made encapsulating the delicate decorative material. First, an intermediate lay-up book is made consisting of the following sequence from top to bottom: (1) four plies of canvas padding; caul plate; (2) textured release paper or plate providing 0.005 inch relief; (3) 0.060 inch clear polymethylmethacrylate sheet (size 48 inches by 96 inches); (4) a layer of the delicate decorative material; (5) 0.060 inch clear polymethylmethacrylate sheet (size 48 inches by 96 inches); (6) textured release paper or plate providing 0.005 inch relief; (7) caul plate; and, (8) four plies of canvas padding. [0053]
  • The press is heated to about 280° F., the intermediate lay-up book is placed in the press, and the press is closed. The pressure is brought to 40 psi. When the materials in the lay-up reach 290° F., the pressure is increased to 160 psi and held for 1 minute. The intermediate product is then gradually cooled to 100° F. [0054]
  • In stage 2, the final lay-up book is made consisting of the following sequence from top to bottom: foul plies of canvas padding; caul plate; textured release paper or plate; 0.060 inch clear polymethylmethacrylate sheet (size 48 inches by 96 inches); 0.12 inch textured intermediate product (from stage 1) encapsulating the delicate decorative material delicate decorative material; 0.060 inch clear polymethylmethacrylate sheet (size 48 inches by 96 inches); textured release paper or plate; caul plate; and, four plies of canvas padding. [0055]
  • The press is preheated to a temperature of about 280° F. Then the final lay-up book is loaded into the press. The press is closed against the book at a pressure of about 40 psi. The press temperature is then ramped tip until the lay-up sandwich reaches a temperature of about 290° F.-310° F. while maintaining the pressure at about 40 psi. The press is opened and all pressure is removed from the book. The press is closed against the book and the pressure is ramped up to about 160 psi. The press temperature is ramped up until the materials in the lay-up sandwich reach a temperature of about 290° F. 15-310° F. while maintaining the pressure at about 160 psi. This pressure and temperature is then held for about 1 to 6 minutes depending on the thickness of the lay-up sandwich to allow the polymethylmethacrylate sheets to melt together in the lay-up sandwich to provide a unitary product. [0056]
  • The heat is then turned off and the product is allowed to gradually cool while maintaining the pressure at about 160 psi until the product reaches a temperature of about 100° F. at which point the press is opened and the product (which may need some trimming) is removed from the press. [0057]
  • Example 2 can also be performed using polyvinyl chloride and polycarbonate, but polycarbonate requires the higher temperature of about 350° F.-375° F. Example 2 can also be performed using a combination of polymethylmethacrylate, polyvinyl chloride, or polycarbonate. [0058]
  • EXAMPLE 3
  • This is an example of the second embodiment of the invention illustrated by FIG. 4. In this example, the basic lay-up sandwich consists of three layers of the following starting materials: (1) a bottom sheet [0059] 22 of the preferred polymethylmethacrylate material that is 0.060 inch thick, 48 inches wide, and 96 inches long; (2) a pre-textured intermediate sheet 24 of the preferred polymethylmethacrylate material that is 0.060 inch thick, 48 inches wide, and 96 inches long; and, (3) a top sheet 26 of the preferred polymethylmethacrylate that is 0.060 inch thick, 48 inches wide, and 96 inches long. When making this product (which does not have a layer of decorative material), it is necessary to pre-texture both surfaces of the intermediate polymethylmethacrylate sheet 24 to allow air and gases to escape during the pressing/heating operation. If the surfaces of the polymethylmethacrylate sheet 24 is not pre-textured, air bubbles will be trapped within the product.
  • In stage 1, an intermediate lay-up book is made consisting of the following sequence from top to bottom: (1) four plies of canvas padding; caul plate; (2) textured release paper or plate providing 0.005 inch relief; (3) 0.060 inch clear or colored polymethylmethacrylate sheet (size 48 inches by 96 inches); (4) textured release paper or plate providing 0.005 inch relief; caul plate; and, (5) four plies of canvas padding. [0060]
  • The press is heated to about 280° F., the intermediate lay-up book is placed in the press, and the press is closed. The pressure is brought to 40 psi. When the lay-up reaches about 290° F., the pressure is increased to 160 psi and held for 1 minute. The intermediate product is then gradually cooled to 100° F. [0061]
  • In stage 2, the final lay-up book is made consisting of the following sequence from top to bottom: (1) four plies of canvas padding; (2) caul plate; (3) textured release paper or plate; (4) 0.060 inch clear polymethylmethacrylate sheet (size 48 inches by 96 inches); (5) 0.060 inch textured intermediate product (from stage I); (6) 0.060 inch clear polymethylmethacrylate sheet (size 48 inches by 96 inches); (7) textured release paper or plate; (8) caul plate; and, (9) four plies of canvas padding. [0062]
  • The press is preheated to a temperature of about 280° F. Then the final lay-up book is loaded into the press. The press is closed against the book at a pressure of about 40 psi. The press temperature is then ramped up until the lay-up sandwich reaches a temperature of about 290° F.-310° F. while maintaining the pressure at about 40 psi. The press is opened and all pressure is removed from the book. The press is closed against the book and the pressure is ramped up to about 160 psi. The press temperature is ramped up until the materials in the lay-up sandwich reach a temperature of about 290° F.-310° F. while maintaining the pressure at about 160 psi. This pressure and temperature is then held for about 1 to 6 minutes depending on the thickness of the lay-up sandwich to allow the polymethylmethacrylate sheets to melt together in the lay-up sandwich to provide a unitary product. [0063]
  • The heat is then turned off and the product is allowed to gradually cool while maintaining the pressure at about 160 psi until the product reaches a temperature of about 100° F. at which point the press is opened and the product is removed from the press. The product has a stratum of the textured material permanently fixated in the matrix and co-extensive with the edges of the matrix. The flat product may be subjected to conventional thermoforming/shaping processes if a non-flat shape is desired. [0064]
  • This Example 3 can also be performed using polyvinyl chloride and polycarbonate, but polycarbonate requires the higher temperature of about 350° F.-375° F. Example 3 can also be performed using a combination of polymethylmethacrylate, polyvinyl chloride, or polycarbonate. [0065]
  • While the preferred embodiments of the invention have been illustrated and described, it will be appreciated that various changes can be made therein without departing from the spirit and scope of the invention. [0066]

Claims (27)

  1. 1. A flat non-porous unitary solid surface structure comprising:
    (a) a flat non-porous unitary matrix made of a polymeric material selected from the group consisting of polymethylmethacrylate, polyvinyl chloride, polycarbonate, and combinations thereof, and
    (b) a visible decorative object that is permanently fixated in the matrix, wherein said decorative object extends to least one edge of said matrix.
  2. 2. The solid surface structure of claim 1 wherein the matrix is made of polymethylmethacrylate.
  3. 3. The solid surface structure of claim 1 wherein the matrix is made of polyvinyl chloride.
  4. 4. The solid surface structure of claim 1 wherein the matrix is made of polycarbonate.
  5. 5. The solid surface structure of claim 1 wherein the decorative object is made of a dry material selected from the group consisting of textile fabric, paper, plastic film, plastic sheet, metallic wire, rod, mesh, bar, wood veneer, dried natural materials, tree bark, plant leaves, petals, and twigs.
  6. 6. The solid surface structure of claim 1 wherein at least one of the outer surfaces of the matrix is embossed or textured.
  7. 7. A flat non-porous unitary solid surface structure comprising:
    (a) a flat non-porous unitary matrix made of polymethylmethacrylate; and
    (b) a visible decorative object that is permanently fixated in the matrix, wherein said decorative object extends to least one edge of said matrix.
  8. 8. The solid surface structure of claim 7 wherein the decorative object is made of a dry material selected from the group consisting of textile fabric, paper, plastic film, plastic sheet, metallic wire, rod, mesh, bar, wood veneer, dried natural materials, tree bark, plant leaves, petals, and twigs.
  9. 9. The solid surface structure of claim 7 wherein at least one of the outer surfaces of the matrix is embossed or textured.
  10. 10. A flat non-porous unitary solid surface structure comprising:
    (a) a flat non-porous unitary matrix made of polyvinyl chloride; and
    (b) a visible decorative object that is permanently fixated in the matrix, wherein said decorative object extends to least one edge of said matrix.
  11. 11. The solid surface structure of claim 10 wherein the decorative object is made of a dry material selected from the group consisting of textile fabric, paper, plastic film, plastic sheet, metallic wire, rod, mesh, bar, wood veneer, dried natural materials, tree bark, plant leaves, petals, and twigs.
  12. 12. The solid surface structure of claim 10 wherein at least one of the outer surfaces of the matrix is embossed or textured.
  13. 13. A flat non-porous unitary solid surface structure comprising:
    (a) a flat non-porous unitary matrix made of polycarbonate; and
    (b) a visible decorative object that is permanently fixated in the matrix, wherein said decorative object extends to least one edge of said matrix.
  14. 14. The solid surface structure of claim 13 wherein the decorative object is made of a dry material selected from the group consisting of textile fabric, paper, plastic film, plastic sheet, metallic wire, rod, mesh, bar, wood veneer, dried natural materials, tree bark, plant leaves, petals, and twigs.
  15. 15. The solid surface structure of claim 13 wherein at least one of the outer surfaces of the matrix is embossed or textured.
  16. 16. A flat non-porous unitary solid surface structure comprising:
    (a) a flat non-porous unitary matrix made of a polymeric material selected from the group consisting of a polymethylmethacrylate, polyvinyl chloride, polycarbonate, and combinations thereof; and
    (b) a visible stratum of textured material made of a material selected from the group consisting of polymethylmethacrylate, polyvinyl chloride, and polycarbonate, wherein said textured material is permanently fixated in the matrix and is co-extensive with the edges of said matrix.
  17. 17. The solid surface structure of claim 16 wherein the matrix is made of polymethylmethacrylate and the visible layer of textured material is made of polymethylmethacrylate.
  18. 18. The solid surface structure of claim 16 wherein the matrix is made of polyvinyl chloride and the visible layer of textured material is made of polyvinyl chloride.
  19. 19. The solid surface structure of claim 16 wherein the matrix is made of polycarbonate and the visible layer of textured material is made of polycarbonate.
  20. 20-39 (Cancelled)
  21. 40. A countertop comprised of the flat non-porous unitary solid surface structure of claim 1.
  22. 41. A sink comprised of the flat non-porous unitary solid surface structure of claim 1.
  23. 42. A lavatory comprised of the flat non-porous unitary solid surface structure of claim 1.
  24. 43. A desktop comprised of the flat non-porous unitary solid surface structure of claim 1.
  25. 44. A table top comprised of the flat non-porous unitary solid surface structure of claim 1.
  26. 45. A chair comprised of the flat non-porous unitary solid surface structure of claim 1.
  27. 46. A windowsill comprised of the flat non-porous unitary solid surface structure of claim 1.
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US6743327B2 (en) 2004-06-01 grant
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US20030113485A1 (en) 2003-06-19 application
CA2490743A1 (en) 2003-10-09 application

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