Classifications

• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
  • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
  • C08J5/18—Manufacture of films or sheets
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
  • B01D67/0002—Organic membrane manufacture
  • B01D67/0023—Organic membrane manufacture by inducing porosity into non porous precursor membranes
  • B01D67/0025—Organic membrane manufacture by inducing porosity into non porous precursor membranes by mechanical treatment, e.g. pore-stretching
  • B01D67/0027—Organic membrane manufacture by inducing porosity into non porous precursor membranes by mechanical treatment, e.g. pore-stretching by stretching
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
  • B01D69/12—Composite membranes; Ultra-thin membranes
  • B01D69/1216—Three or more layers
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
  • B01D71/06—Organic material
  • B01D71/72—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, not provided for in a single one of the groups B01D71/46 - B01D71/70 and B01D71/701 - B01D71/702
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
  • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
  • B29C55/00—Shaping by stretching, e.g. drawing through a die; Apparatus therefor
  • B29C55/005—Shaping by stretching, e.g. drawing through a die; Apparatus therefor characterised by the choice of materials
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
  • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
  • B29C55/00—Shaping by stretching, e.g. drawing through a die; Apparatus therefor
  • B29C55/02—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets
  • B29C55/023—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets using multilayered plates or sheets
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
  • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
  • B29C55/00—Shaping by stretching, e.g. drawing through a die; Apparatus therefor
  • B29C55/02—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets
  • B29C55/10—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial
  • B29C55/12—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial biaxial
  • B29C55/16—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial biaxial simultaneously
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
  • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
  • B29C67/00—Shaping techniques not covered by groups B29C39/00 - B29C65/00, B29C70/00 or B29C73/00
  • B29C67/20—Shaping techniques not covered by groups B29C39/00 - B29C65/00, B29C70/00 or B29C73/00 for porous or cellular articles, e.g. of foam plastics, coarse-pored
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
  • B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
  • B29D7/00—Producing flat articles, e.g. films or sheets
  • B29D7/01—Films or sheets
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
  • C08G61/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
  • C08G61/02—Macromolecular compounds containing only carbon atoms in the main chain of the macromolecule, e.g. polyxylylenes
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
  • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
  • C08J7/04—Coating
  • C08J7/042—Coating with two or more layers, where at least one layer of a composition contains a polymer binder
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
  • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
  • C08J7/04—Coating
  • C08J7/0427—Coating with only one layer of a composition containing a polymer binder
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
  • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
  • C08J9/22—After-treatment of expandable particles; Forming foamed products
  • C08J9/228—Forming foamed products
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
  • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
  • C08J9/36—After-treatment
  • C08J9/365—Coating
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L65/00—Compositions of macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain; Compositions of derivatives of such polymers
  • C08L65/04—Polyxylenes
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
  • C09D165/00—Coating compositions based on macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain; Coating compositions based on derivatives of such polymers
  • C09D165/04—Polyxylylenes
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
  • B01D71/06—Organic material
  • B01D71/30—Polyalkenyl halides
  • B01D71/32—Polyalkenyl halides containing fluorine atoms
  • B01D71/36—Polytetrafluoroethene
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
  • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
  • B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
  • B29K2105/04—Condition, form or state of moulded material or of the material to be shaped cellular or porous
  • B29K2105/041—Microporous
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
  • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
  • B29K2865/00—Use of polyphenylenes or polyxylylenes as mould material
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
  • C08G2261/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
  • C08G2261/30—Monomer units or repeat units incorporating structural elements in the main chain
  • C08G2261/34—Monomer units or repeat units incorporating structural elements in the main chain incorporating partially-aromatic structural elements in the main chain
  • C08G2261/342—Monomer units or repeat units incorporating structural elements in the main chain incorporating partially-aromatic structural elements in the main chain containing only carbon atoms
  • C08G2261/3424—Monomer units or repeat units incorporating structural elements in the main chain incorporating partially-aromatic structural elements in the main chain containing only carbon atoms non-conjugated, e.g. paracyclophanes or xylenes
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
  • C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
  • C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
  • C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
  • C08J2327/18—Homopolymers or copolymers of tetrafluoroethylene
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
  • C08J2365/00—Characterised by the use of macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain; Derivatives of such polymers
  • C08J2365/04—Polyxylylenes
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
  • C08J2465/00—Characterised by the use of macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain; Derivatives of such polymers
  • C08J2465/04—Polyxylylenes

Definitions

• the present invention relates generaiiy to polyparaxylylene, and more specifically to porous articles containing polyparaxylylene polymers where the articles have a node and fibril structure.
• a process for the formation of porous articles from polyparaxylylene polymers is also provided.
• Polyparaxylylene (PPX) and its derivatives are well known in the art. Artides made from PPX possess physical properties such as resistance to chemical attack, resistance to gamma radiation, thermo-oxidative stability at elevated temperatures, biocompatibility, high dielectric strength, high mechanical strength, and excellent barrier properties. Because of the favorable attributes associated with it, PPX has been utilized as a monolithic coating or film in a variet of applications including thin film dielectrics, electrical insulation, chemical resistance, and barrier coatings.
• PPX polymers cannot be made into useful forms by conventional processing routes such as compression molding, extrusion, solvent casting, gel spinning, or sintering because there is no melt state or solution state.
• porous PPX articles have been made through the addition of porogens, by coating a porous scaffold composed of another polymer, and fay thermal exposure that causes degradation of the PPX polymer introducing localized holes.
• One embodiment relates to a process for forming a porous
• polyparaxyiylene article that includes (1) depositing a poiyparaxyiylene (PPX) polymer film on a first side and a second side of a substrate to form a PPX composite structure and (2) expanding the PPX composite structure to form a first porous PPX polymer article on the first side of the substrate and a second porous PPX polymer article on the second side of the substrate.
• PPX poiyparaxyiylene
• Each of the porous PPX polymer articles have a node and fibril structure.
• the process further includes removing at least one of the porous PPX polymer articles from the substrate.
• the PPX polymer films have a thickness less than about 50 microns.
• the PPX composite structure may be expanded at a temperature from about 80°C to about 450°C, or from 220°C to about 450°C. Polymer chains in the fibrils are oriented along a fibril axis. In at least one embodiment, PPX is deposited onto the first and second sides of the substrate by vapor deposition.
• the substrate is a substrate that is capable of substantia! deformation.
• a second embodiment relates to a porous polyparaxyiylene (PPX) polymer article that includes (1) a substrate having a first side and a second side, (2) a first expanded PPX polymer film on the first side of the substrate, and (3) a second expanded PPX polymer film on the second side of the substrate,
• the porous PPX polyme article includes nodes and fibrils.
• the fibriis include polymer chains oriented along a fibril axis.
• the substrate may be an expanded
• ePTFE polytetrafSuoroethylene
• PTFE polytetrafluoroethylene
• ePTFE membrane a polytetrafluoroethylene (PTFE) tape
• PTFE membrane a polytetrafluoroethylene (PTFE) membrane
• ePTFE membrane an expanded po!ytetrafluorethylene (ePTFE) tape
• poiyimide poiyimide
• polyamide-imide silicon, glass, or zinc
• a third embodiment relates to a process for forming a porous polyparaxyiylene article that includes (1) forming a polyparaxyiylene (PPX) compostte article and (2) expanding the PPX composite article to form a porous PPX polymer article having a node and fibril structure.
• the composite article is formed by (1) depositing a first PPX polymer film on a first side of a substrate and (2) forming a second PPX polymer film on the second side of the substrate.
• the PPX polymer films have a thickness less than about 50 microns, in some embodiments, the first PPX polymer film has a microstructure that is different from the microstructure of th second PPX polymer film. In other embodiments, the microstructures of the first and second PPX polymer films are the same or substantially the same.
• FIG. 1 is a scanning electron micrograph (SE ) of the surface of the non-expanded, non-porous polyparaxylylene-AF4 film of the Comparative Example taken at 5,000x magnification;
• [ ⁇ ] FiG. 2 is a scanning electron micrograph (SEM) of the cross-section of the non-expanded:, non-porous poiyparaxylylene-AF4 film of the Comparative Example taken at 5,000x magnification;
• FIG. 3 is a scanning electron micrograph (SEM) of the surface of the expanded porous polyparaxylylene-AF4 membrane of Example 1 taken at 50,000x magnification where the machine direction (MD) is horizontal in accordance with one embodiment of the invention;
• FIG. 4 is a scanning electron micrograph (SEM) of the cross-section of the expanded porous po!yparaxyiylene-AF4 sheet of Example 1 taken at 1 ,000x magnification in accordance with one embodiment of the invention;
• FIG . 5 is a wide angle x-ray diffraction (WAXD) pattern of the non- expanded, non-porous polyparaxylylene ⁇ AF4 film of the Comparative Example;
• WAXD wide angle x-ray diffraction
• FIG. 6 is wide angle x-ray diffraction (WAXD) pattern of the biaxially expanded porous polyparaxyiylene-AF4 membrane of Example 1 with the machine direction oriented in the vertical direction according to at least one embodiment of the invention;
• WAXD wide angle x-ray diffraction
• FIG. 7A is a scanning electron micrograph (SEM) of the surface of the expanded porous polyparaxy!yJene ⁇ AF4 article of Example 3 taken at 20,000x magnification in accordance with an embodiment of the invention
• FIG. 7B is a scanning electron micrograph (SEM) of the surface of the expanded porous expanded porous poiyparaxy!ylene-AF4 article of Example 3 taken at 5000x magnification according to at least one embodiment of the invention;
• FIG. 8 is a scanning electron micrograph (SEM) of the surface of the expanded pofyparaxylylene-AF4 article of Example 6 taken at 20,000x magnification in accordance with an embodiment of the invention
• F'G- 9 is a scanning electron micrograph (SEM) of the surface of the expanded pQiyparaxyly!ene-AF4 article of Example 9 taken at 45,000x magnification according to at least one embodiment of the invention
• FIG. 10 is a scanning electron micrograph (SEM) of the surface of the PPX-N membrane of Example 11 drawn to an extension ratio of 2,2 at an
• FIG. 11 is a scanning electron micrograph (SEM) of the PPX-N fine powder of Example 12 taken at 4,000x magnification according to at least one embodiment of the invention
• F!G. 12 is a differentia! scanning thermogram (DSC) of the non- expanded, non-porous PPX-AF4 membrane of the Comparative Example.
• FIG. 13 is a differential scanning thermogram (DSC) of the expanded, porous PPX-AF4 membrane of Example 1 according to an embodiment of the invention.
• FIG. 14 is a scanning electron micrograph (SEM) of the surface of the co-expanded PTFE/PPX-AF4 membrane of Example 14 taken at 40,000x
• FIG , 15 is a scanning electron micrograph (SEM) of the cross-section of the co-expanded PTFE/PPX-AF4 membrane of Example 1 taken at 3000x magnification in accordance with one embodiment of the invention;
• FIG. 16 is a scanning electron micrograph (SEM) of the cross-section of the expanded PTFE/PPX-AF4 composite article of Example 16 taken at 500x magnification in accordance with one embodiment of the invention.
• FIG. 17 is a scanning electron micrograph (SEM) of the cross-section of the expanded PTFE/PPX-AF4 composite article of Example 16 taken at 500x magnification according to an embodiment.
• PPX polyparaxylylene
• PPX polymer is meant to include ail forms of PPX, including PPX-N, PPX-AF4, PPX-VT4, and combinations thereof.
• PPX polymer film as used herein is meant to denote unexpended PPX polymer, either free-standing or on a substrate, (60030]
• PPX polymer membrane as used herein is meant to denote a PPX polymer film that has been expanded in one or more directions,
• PPX composite structure as used herein is meant to describe a PPX polymer film that has been formed on one or both sides of a substrate
• a porous PPX polymer article is meant to denote an expanded PPX polymer film (e.g. , PPX polymer membrane), either free-standing or as a co-expanded PPX poiymer film/substrate or a co-expanded PPX polymer filrn/substrate/PPX. polymer film.
• expanded PPX polymer film e.g. , PPX polymer membrane
• lubricant is meant to describe a processing aid that includes, and in some embodiments, consists of, an incompressible fluid that is not a solvent for the polymer at processing conditions, The fluid-polymer surface interactions are such that it is possible to create a homogenous mixture.
• extension ratio is meant to define strain as the final length divided by the original length.
• node is meant to describe the connection point of at least two fibrils.
• the term "thin” is meant to describe a thickness of less than about 50 microns.
• fibril axis is meant to describe direction parallel to the long dimension of the fibril.
• substantially deformation is meant to describe a substrate that is capable of elongating in one or more direction without breaking.
• the present invention relates to poiyparaxyly!ene (PPX) poiymers that can be expanded into porous articles that have a node and fibril mtcrostructure.
• the fibrils contain PPX polymer chains oriented with the fibril axis,
• the PPX polymer may contain one or more comonomer.
• PPX polymer is meant to include all forms of PPX, including PPX- N, PPX-AF4, PPX-VT4, and combinations thereof.
• PPX may be applied to one or both sides of a substrate, such as by any conventional vapor deposition method.
• the substrate is not particularly limiting so iong as the substrate is dimensionaily stable and the PPX polymer film formed thereon can be removed from the substrate, if desired.
• suitable substrates include a
• PTFE polytetrafiuoroethytene
• ePTFE polytetraftuorethylene
• the substrate is capable of substantial deformation in one or more directions, such as a PTFE film or
• the PPX polymer film may have a nominal thickness less than about 50 microns, in exemplary
• the PPX polymer film has a thickness from about 0.1 microns to about 50 microns, from about 0.1 microns to about 40 microns, from about 0.1 microns to about 30 microns, from about 0, 1 microns to about 20 microns, from about 0.1 microns to about 10 microns, from about 0, 1 microns to about 5 microns, from about 0, 1 microns to about 2 microns, or from about 0.1 microns to about 1 micron.
• a thin PPX polymer film on one side of a substrate for example a PTFE substrate
• a substrate for example a PTFE substrate
• the PPX polymer film on one side of the substrate may or may not have the same microstructure as the PPX polymer film on the opposing side of the substrate. If the PPX polymer films have different microstructures, the composite structure contains three different microstructures, If the PPX polymer films have the same microstructure (or substantiall the same microstructure such that the microstructures cannot be distinguished from each other), the composite structure contains two different microstructures.
• the difference between the first mi.cFOstructu.re, the second micro-structure, and the third microstructure can be measured by, for example, a difference in pore size (porosity), a difference in node and/or fibril geometry or size, and/or a difference in density, ft is to be appreciated thai the composite structure may include additional PPX polymer fllm(s) and/or substrate(s) and may therefore have more than three microstructures within the composite structure,
• the PPX polymer film ⁇ s) may be removed from the substrate to form a free-standing PPX polymer fifm(s).
• the free-standing PPX polymer film may be stretched or expanded in one or more directions to form a porous PPX membrane.
• a PPX composite structure e.g. , th PPX polymer fiim(s) on a substrate
• may be co-expanded in one or more directions to form a porous PPX poiymer article e.g. , co-expanded PTFE/PPX membrane or co-expanded PPX polymer film /PTFE/PPX polymer film.
• the expanded PPX polymer may be removed from the expanded substrate to form a free standing expanded PPX poiymer membrane ⁇ s).
• the expanded PPX polymer membrane may be referred to herein as a porous PPX polymer article, it is to be noted that the expanded composite structure (e.g., the expanded PPX polymer film/expanded substrate or expanded PPX polymer film/expanded substrate/expanded PPX polymer film) may remain as a singie unit in some embodiments, in other embodiments, a PPX polymer film is deposited on one or both sides of a substrate and co-expanded into a PPX composite structure, after which one or both of the expanded PPX poiymer films Is removed.
• a PPX polymer film(s) may be deposited onto a partially expanded substrate, such as a partiaiiy expanded PTFE tape o membrane.
• the PPX polymer fllm(s) and the partially expanded substrate may then be co-expanded.
• the expanded PPX poiymer film(s) may be removed from the expanded substrate to become a free-standing PPX expanded poiymer membrane or porous PPX article.
• the PPX polymer film (with or without an expandable substrate) may be cut into suitable sizes for expansion. Expansion of the free-standing PPX polymer film(s) occur at a temperature from about 80°C to about 220°C or from about 22Q°C to about 290°C or from about 290°C to about 450°C.
• Expansion of a composite structure of a PPX poiymer fs!m/PTFE substrate or PPX polymer fflm/PTFE substrate/PPX polymer film may occur at temperatures from about 80°C to about 220X, from about 220°C to about 340X, or from about 290X to about 340°C (i.e., below the melt temperature of the PTFE substrate). It is to be noted that the maximum temperature for expanding any composite structure described herein is the temperature at which the substrate degrades or melts. Expansion may be conducted at engineering strain rates (ESR) up to 10,000%/second, or from 1% to 10,000%/ second or from 10% to 5000%/second to form an expanded, porous PPX article.
• ESR engineering strain rates
• the expanded PPX membrane has a microstructure of nodes interconnected by fibrils, optionally with regions of unexpanded PPX, such as may be seen in FIGS.3, 4, 7, 8, 9 and 10.
• FIGS. 4 and 78 fo example, show expanded regions 40 and unexpanded regions 50 in the expanded PPX membranes.
• the microporous structure and the geometry of the interconnected fibrils can be controlled by the deposition conditions, the rate of expansion, temperature of expansion, and ultimate expansion ratio in each direction.
• FIG. 5 a wide angle x-ray diffraction (WAXD) pattern consistent with highly crystalline, randomly oriented lamella of the unexpanded or as-deposited PPX sample is depicted.
• WAXD wide angle x-ray diffraction
• FIG. 8 the WAXD pattern of an expanded PPX article oriented with the larger expansion in the vertical direction is depicted in FIG. 8, which shows a new diffraction peak at reference numeral 30.
• This WAXD pattern shows an emergence of two additional equatorial reflections (at 3 o'clock and 9 o ' clock) in a d-spacing of about 0.45 nm and two distinct meridonal reflections (at 12 o'clock and 6 o'clock) in a d-spacing of about 0.32 nm.
• These reflections are associated with oriented polymer chains in the fibrils in the expanded PPX article. In other words, the polymer chains in the fibrils are oriented along the fibril axis.
• the expanded PPX article would display a WAXD pattern illustrating an additional signal at the 0.45 nm d-spacing, which may show up as additional diffraction spots or a concentric ring.
• the expanded PPX articles are porous, and may have a percent porosity of at least about .5%, at least about 10%, at least about 15%, at least about 20%, at least about 25%, at least about 30%, at least about 35%, at least about 40%, at least about 45%, at least about 50%, ai least about 55%, at least about 60%, at least about 65%, at least about 70%, at least about 75%, at least about 80%, at least about 85%, or up to (and: including) 90%.
• the expanded PPX articles may have a percent porosity from about 5% to about 75%, from about 10% to about 50%, or from about 10% to about 25%.
• a porous PPX article may be formed from a crystalline PPX polymer in the form of a powder.
• PPX polymer and a lubricant are mixed so as to uniformly or substantially uniformly distribute the lubricant in the mixture.
• lubricant is meant to describe a processing aid that is an incompressible fluid that is not a solvent for the polymer at the process conditions, The fluid-polymer surface Interactions are such that it is possible to create a homogenous mixture, it is also to be noted that that choice of lubricant is not particularly limiting and the selection of lubricant is largely a matter of safety and convenience.
• Non-limiting examples of lubricants for use herein include light mineral oil, aliphatic
• hydrocarbons aromatic hydrocarbons, haiogenafed hydrocarbons, and the like, and may be selected according to fiammabiiity, evaporation rate, and economic considerations.
• the lubricated PPX polymer is heated to a temperature about 80°C to about 22Q°C or from about 220°C to about 290°C or from about 29G°C to about 450"C.
• the lubricated PPX polymer is heated to at a temperature from about 220°C and below the temperature at which the polymer would decompose during processing, and in exemplar embodiments, from about 220°C to about 250°C ⁇ in an inert atmosphere).
• sufficient pressure and shear is applied so as to form inter-particle connections and create a solid form.
• methods of applying pressure and shear include ram extrusion ( ⁇ , ⁇ ?., typically called paste extrusion or paste
• the lubricated PPX polymer is calendered or ram extruded to produce a cohesive sheet that may be used as a preform.
• cohesive is meant to describe a sheet that is sufficiently strong for further processing.
• the calendering or ram extrusion occurs at a temperature about 80°C to about 220X or from about 220°C to about 290°C or from about 290 e C to about 450°C
• the calendering or ram extrusion occurs from about 220° ' C and below the temperature at which the polymer would decompose during processing, and in exemplary embodiments, from about 220°C to about 250°C (in an inert atmosphere)
• the lubricated PPX polymer may be ram extruded to produce a cohesive sheet, tube, or cylinde preform, in either calendering or ram extruding, the PPX polymer preform may be subsequently expanded as described above to form a porous PPX polymer article.
• SElvl images were collected using an Hitachi SU8000 FE Ultra High Resolution Scanning Electron Microscope with Dual SE detectors.
• Cross-sectioned samples were prepared using a Cooled straight-razor blade method. Surface and cross-sectioned samples were mounted onto a 25 mm diameter mefai stub with a 25 mm carbon double sided adhesive. The mounted samples were sputter coated with platinum.
• WAXD W de Angle X-ray Diffraction
• Diffraction patterns from as-deposited and expanded films were collected using a Molecular Metrology instrument configured for 2-D WAXD observations.
• the X-Ray source was a Rigaku icro ' Max Sealed Micro Source CuKa element with a wavelength of 0.1542 nm running at 45 kV/66 mA.
• To collect two- dimensional diffraction information at wide angles a 20 cm x 20 cm Fujifiim BAS SR2040 imaging plate was placed in the instrument vacuum chamber perpendicular to the X-Ray beam line at a camera length of 146 mm.
• Diffraction patterns from calendered PPX powder were collected using a Bruker Discovery D-8 instrument.
• the X-Ray source was CuKa element with a wavelength of 0.1542 nm running at 40 kV/60 mA.
• the instrument was configured in a Srentano-Bragg geometry. Diffraction intensity was measured using a OD scintillation counter rotating at 0.0.2 degree 2-theta increments for a one second duration. The range of 2-theta was 10 degrees to 45 degrees.
• the instrument was calibrated using a polycrystaine silicon and an automated interna! calibration algorithm.
• a PPX polymer was placed on the Bruker Discovery D-8 stage and aligned with the beam line.
• the Gurle air flow test measures the time in seconds for 100 cm 3 of air to flow through a 6.45 cm 2 aperture at 12.4 cm of water pressure. If the sample size was smaller than 6.45 cm 2 an aperture of 0.645 cm 2 was used and the time observed divided by a factor of 10 to normalize observations made with both apertures. The samples were measured in a Gurley Densometer Model 4110 Automatic Densometer equipped with a Gurley Model 4320 automated digital timer. The reported results are the average of multiple (3-5) measurements.
• DSC data were coilected using a TA Instruments Q2000 DSC between 0°C and 425°C using a heating and a cooling rate of 10 °G/min.
• the expanded porous membrane samples and the solid film samples were prepared by punching out .4 mm disks.
• the 4 mm disk was placed flat n the pan and the ltd was crimped to sandwich the disk between the pan and lid.
• a film of PPX-AF4 having a nominal thickness of 10 pm was deposited onto a blended, extruded, and dried PTFE tape made generally in accordance with the teachings of U.S. Patent No. 3,953,566 to Gore by a commercially available vapor deposition process (Specialty Coating Systems, 7645 Woodland Drive,
• the coated article was then cut to dimensions of 200 mm x 200 mm and placed i the grips of a pantograph type biaxial batch expander equipped with a convection oven.
• the coated tape was heat soaked at a constant temperature of 35Q°C for 300 seconds.
• the heat treated article was aiowed to cool to room temperature under restraint of the pantograph biaxial expander grips.
• the PPX-AF4 film was removed from the melted PTFE carrier tape to yield a free-standing, non-expanded, non- porous film of PPX-AF4.
• a scanning electron micrograph (SE ) of the surface and cross- section of the non-expanded, non-porous PPX-AF4 film are shown in FIGS, 1 and 2, respectively.
• a wide angle x-ray diffraction (WAXD) pattern of the PPX-AF4 film is shown in FIG. 5.
• a differential scanning thermogram (DSC) of the PPX-AF4 film is shown in FIG. 12, As shown in FIG, 12, the non-expanded, non-porous PPX-AF4 film, on cooling, exhibits a single exothermic peak at approximately 3S0°C.
• a Gurley number of the non-expanded, non-porous PPX AF4 film was determined to be greater than 3600 seconds and is reported in Table 1.
• a film of PPX-AF4 having a nominal thickness of 10 pm was deposited onto a blended, extruded, and dried PTFE tape made generally in accordance with the teachings of U.S. Patent No. 3,953,566 to Gore by a
• the coated article was then cut to dimensions of 200 mm x 200 mm and placed in the grips of a pantograph type biaxial batch expander equipped with a convection oven.
• the coated tape was heat soaked at a constant temperature of 350°C for 300 seconds.
• the coated tape was then simultaneously stretched at an engineering strain rate (ESR) of 100 percent/second to an extension ratio in the tape machine direction of 1:1 and 4:1 in the tape transverse direction.
• ESR engineering strain rate
• the expanded article was allowed to coo! to room temperature under restraint of the pantograph biaxial expander grips. After cooling, the article was removed from the expander grips and a film of porous PPX-AF4 was removed from the melted PTFE tape to yield a free-standing porous membrane of PPX-AF4.
• FIGS. 3 and 4 Scanning electron micrographs (SEI Is) of the surface and the cross* section of the expanded porous PPX-AF4 membrane are shown in FIGS. 3 and 4, respectively.
• a wide angle x-ray diffraction (WAXD) pattern of the expanded porous PPX-AF4 membrane is shown in FIG. 6.
• a differential scanning: thermogram (DSC) of the expanded , porous PPX-AF4 membrane is shown in FIG. 13.
• DSC thermogram
• FIG. 13 the free-standing expanded, porous PPX-AF4 membrane, on cooling, exhibits two exothermic peaks, namely a first peak at 378.8°C and the second peak at 401 ,36°C.
• Gurley number of the expanded PPX-AF4 membrane was determined to be 127.5 seconds and is reported in Table 1.
• a film of PPX-AF4 having a nominal thickness of 5 pm was deposited onto a blended, extruded, and dried poiytetrafiuoroethylene (PTFE) tape made generally in accordance with the teachings of U.S. Patent No. 3,953.566 to Gore by a commercially available vapor deposition process (Specialty Coating Systems, 7645 Woodland Drive, Indianapolis, IN 46278).
• PTFE poiytetrafiuoroethylene
• T e coated article was then cut to dimensions of 200 mm x 200 mm and placed in the grips of a pantograph type biaxial batch expander equipped with a convection oven.
• the coated tape was heat soaked at a constant temperature of 300°C for 300 seconds.
• the coated tape was then simultaneously stretched at an engineering strain rate (ESR) of 7 percenf second to an extension ratio in the extrudate machine direction of 4: 1 and 4: 1 in the extrudafe transverse direction.
• ESR engineering strain rate
• a film of PPX-AF4 having a nominal thickness of S pm was deposited onto a blended, extruded, and dried poiytetrafluoroethyiene (PTFE) tape made generally in accordance with the teachings of U.S. Patent No. 3,953,568 to Gore by a commercially available vapor deposition process (Specialt Coating Systems, 7645 Woodland Drive, Indianapolis, IN 46278).
• the coated article was then cut to dimensions of 200 mm x 200 mm and placed in the grips of a pantograph type biaxial batch expander equipped with a convection oven.
• the coated tape was heat soaked at a constant temperature of 300°C for 300 seconds.
• the coated tape was then simultaneously stretched at an engineering strain rate (ES ) of 70
• the expanded PPX-AF4 article was removed from the oven and allowed to cool to room temperature under restraint of the biaxial batch expander grips. After cooling, the expanded PPX-AF4 article (i.e. , co-expanded PTFE/PPX-AF4 membrane) was removed from the grips.
• FIG. 7A A scanning electron micrograph (SE ) of the surface of the expanded PPX-AF4 membrane taken at 20,000x magnification is shown in FIG. 7A, A representative node is depicted by reference numeral 10 and a representative fibril is depicted by reference numeral 20.
• F!G. 7B is an SEM of the surface of the expanded PPX-AF4 membrane taken at SOOOx magnification depicting therein an expanded region 40 and an unexpanded region 50.
• a Gurley number of the expanded PPX-AF4 article was determined to be 89.1 seconds and is reported in Table 1.
• a film of PPX-AF4 having a nominal thickness of 5 um was deposited onto a b!ended, extruded, and dried poiytetrafluoroethyiene (PTFE) tape made generally in accordance with the teachings of U.S. Patent No, 3,953,566 to Gore by a commercially available vapor deposition process ⁇ Specialty Coating Systems, 7645 Woodland Drive, Indianapolis, IN 46278).
• PTFE poiytetrafluoroethyiene
• the coated article was then cut to dimensions of 200 mm x 200 mm and placed in the grips of a pantograph type biaxial batch expander equipped with a convection oven.
• the coated tape was heat soaked at a constant temperature of 300°C for 300 seconds.
• the coated tape was then simultaneously stretched at an engineering strain rate (ESR) of 700 percent/second to an extension ratio in the extrudate machine direction of 4:1 and 4:1 in the tape transverse direction.
• ESR engineering strain rate
• the expanded PPX-AF4 article was removed from the oven and owed to cool to room temperature under restraint of the biaxial batch expander grips. After cooling, the expanded PPX-AF4 article ⁇ i.e., co-expanded PTFE/PPX-AF4 membrane) was removed from the grips.
• a Gurley number of the expanded PPX-AF4 article was determined to be 111.7 seconds and is reported in Table 1.
• a film of PPX-AF4 having a nominal thickness of 5 pm was deposited onto a blended, extruded, and dried po!ytetrafluoroethylene (PTFE) tape made generally in accordance with the teachings of U.S. Patent No. 3,953,566 to Gore by a commercially available vapor deposition process (Specialty Coating Systems, 7645 Woodland Drive, Indianapolis, IN 46278).
• PTFE polytetrafluoroethylene
• the coated article was then cut to dimensions of 200 mm x 200 mm and placed in the grips of a pantograph type biaxial batch expander equipped with a convection oven.
• the coated tape was heat soaked at a constant temperature of 300°C for 300 seconds,
• the coated tape was then simultaneously stretched at an engineering strain rate (ESR) of 7 percent second to an extension ratio in the extrudate machine direction of 6:1 and 6:1 in the tape transverse direction.
• ESR engineering strain rate
• the expanded PPX-AF4 article was removed from the oven and allowed to coo! to room temperature under restraint of the pantograph biaxial expander grips.
• the expanded PPX-AF4 article i.e. , co-expanded PTFE/PPX-AF4 membrane
• a Gurley number of the expanded PPX-AF4 article was determined to be 60.92 seconds and is reported in Table 1.
• a film of PPX-AF4 having a nominal thickness of 5 pm was deposited onto blended, extruded, and dried polytetrafluoroethylene (PTFE) tape made generally in accordance with the teachings of U.S. Patent No. 3,953,566 to Gore by a commercially available vapor deposition process ⁇ Specialty Coating Systems, 7645 Woodland Drive, Indianapolis, IN 46278).
• PTFE polytetrafluoroethylene
• the coated article was then cut to dimensions of 200 mm x 200 mm and placed in the grips of a pantograph type biaxial batch expander equipped with a convection oven.
• the coated tape was heat soaked at a constant temperature of 300°C for 300 seconds.
• the coated tape was then simultaneously stretched at an engineering strain rate (ESR) of 70 percent/second to an extension ratio in the tape machine direction of 6:1 and 6:1 in the tape transverse direction.
• ESR engineering strain rate
• a film of PPX-AF4 having a nominal thickness of 5pm was deposited onto a blended, extruded, and dried polytetrafluoroethylene (PTFE) tape made generally in accordance with the teachings of U.S. Patent No. 3,953,566 to Gore by a commercially available vapor deposition process ⁇ Specialty Coating Systems, 7645 Woodland Drive, Indianapolis, IN 46278).
• PTFE polytetrafluoroethylene
• the coated article was then cut to dimensions of 200 mm x 200 mm and placed in the grips of a pantograph type biaxial batch expander equipped with a convection oven.
• the coated tape was heat soaked at a constant temperature of 300°C for 300 seconds.
• the coated tape was then simultaneously stretched at an engineering strain rate (ESR) of 700 percent/second to an extension ratio in the extrudate tape machine direction of 6:1 and 6:1 in the tape transverse direction.
• ESR engineering strain rate
• the expanded PPX-AF4 article was removed from the oven and allowed to cool to room temperature under restraint of the biaxial batch expander grips.
• the expanded PPX-AF4 article ⁇ i.e., co-expanded PTFE/PPX-AF4 membrane) was removed from the grips.
• a Guriey number of the expanded PPX-AF4 article was determined to be 85,06 and is reported in Table 1.
• a film of PPX-AF4 having a nominal thickness of 5 ⁇ was deposited onto blended, extruded, and dried poiytetrafluoroethyiene (PTFE) tape made generally in accordance wit the teachings of U.S. Patent No. 3,953,566 to Gore by a commercially available vapor deposition process (Specialty Coating Systems, 7645 Woodland Drive, Indianapolis, IN 46278).
• PTFE poiytetrafluoroethyiene
• the coated article was then cut to dimensions of 200 mm x 200 mm and placed i the grips of a pantograph type biaxial batch expander equipped with a convection oven.
• the coated tape was heat soaked at a constant temperature of 250°C for 300 seconds.
• the coated tape was then simultaneously stretched at an engineering strain rate (ESR) of 7 percent/second to an extension ratio in the tape machine direction of 4:1 and 4:1 in the tape transverse direction.
• ESR engineering strain rate
• a film of PPX-AF4 having a nominal thickness of 5 pm was deposited onto a blended, extruded, and dried poiytetrafluoroethyiene (PTFE) tape made generally in accordance with the teachings of U.S. Patent No. 3,953,566 to Gore by a commercially available vapor deposition process (Specialty Coating Systems, 7645 Woodland Drive, Indianapolis, IN 46278).
• PTFE poiytetrafluoroethyiene
• the coated article was then cut to dimensions of 200 mm x 200 mm and placed in the grips of a pantograph type biaxial batch expander equipped with a convection oven.
• the coated tape was heat soaked at a constant temperature of 250°C for 300 seconds.
• the coated tape was then simultaneously stretched at an engineering strain rate (ESR) of 70 percent second to an extension ratio in the tape machine direction of 6: 1 and 6:1 in the tape transverse direction.
• ESR engineering strain rate
• FIG. 9 is a scanning electron micrograph (SEM) of the surface of the expanded PPX-AF4 article of taken at 45,00Qx magnification showing a fibriilated region.
• SEM scanning electron micrograph
• a film of PPX-AF4 having a nominal thickness of 5 pm was deposited onto a blended, extruded, and dried pofytetrafluoroethylene (PTFE) tape made generally in accordance with the teachings of U.S. Patent No. 3,953,566 to Gore by a commercially available vapor deposition process (Specialty Coating Systems, 7645 Woodland Drive, Indianapolis, IN, 46278).
• PTFE pofytetrafluoroethylene
• the coated article was then cut to dimensions of 200 mm x 200 mm and placed in the grips of a pantograph type biaxial batch expander equipped with a convection oven.
• the coated tape was heat soaked at a constant temperature of 250°C for 300 seconds.
• the coated tape was then simultaneously stretched at an engineering strain rate (ESR) of 700 percent/second to an extension ratio in the tape machine direction of 6:1 and 6: 1 in the tape transverse direction.
• ESR engineering strain rate
• a film of PPX-N having a nominal thickness of 10 pro was deposited onto a blended, extruded, and dried polytetrafluoroethylene (PTFE) tape made generally in accordance with the teachings of U.S. Patent No. 3,953,566 to Gore by a commercially available vapor deposition process ⁇ .Specialty Coating Systems, 7645 Woodland Drive, Indianapolis, IN 46278).
• PTFE polytetrafluoroethylene
• the coated article was then cut into a 35 rnm x 13 mm rectangle with the samples long dimension aligned with the ExampSe 1 tape machine direction (MD) direction.
• MD ExampSe 1 tape machine direction
• the rectangular sample was drawn to an extension ratio of 2.2 at an engineering strain rate (ESR) of 50 percent per second in a RSA 3 Dynamic
• FIG. 11 is a scanning electron micrograph (SEM) of the PPX-N powder taken at 4,G00x magnification.
• the PPX-N powder of Example 12 was lubricated with mineral oil and calendered at 150°C to form a thin PPX-N sheet about 0,5 mm thick.
• a film of PPX-AF4 having a nominal thickness of 10 pm was deposited onto a blended, extruded, and dried polytetrafiuoroethylene (PTFE) tape made generally in accordance with the teachings of U.S. Patent No. 3,953,568 to Gore by a commercially available vapor deposition process (Specialty Coating Systems, 7645 Woodland Drive, Indianapolis, IN 46278).
• PTFE polytetrafiuoroethylene
• the coated article was then simultaneously stretched at an engineering strain rate (ESR) of 100 percent/second to an extension ratio of 2:1 in both the extrudate machine and transverse directions.
• ESR engineering strain rate
• the expanded PPX-AF4 article was removed from the oven, and allowed to cool to room temperature under restraint of the biaxial batch expander grips. After cooling, the co-expanded
• FIG. 15 shows a scanning electron micrograph (SEW) of the cross-section of the above co-expanded PTFE/PPX-AF4 membrane taken at 3000x magnification.
• SEW scanning electron micrograph
• a film of PPX-AF4 having a nominal thickness of 5 pm was deposited onto the external surfaces of a blended, extruded, and dried poiytetrafluoroethylene (PTFE) tape made generally in accordance with the teachings of U.S. Patent No. 3,953,566 to Gore by a commercially available vapor deposition process (Specialty Coating Systems, 7645 Woodland Drive, Indianapolis, IN 46278,
• the coated article was then cut to dimensions of 200 mm x 200 mm and placed in the grips of a pantograph type biaxial batch expander equipped with a convection oven.
• the coated tape was heat soaked at a constant temperature of 335°C for 300 seconds.
• the coated tape was then simultaneously stretched at an engineering strain rate (ESR) of 10 percent second to an extension ratio in the extrudate machine direction of 2: 1 and 2: 1 in the extrudate transverse direction.
• ESR engineering strain rate
• the article was then heat soaked at a constant temperature of Z Q°C for 30 seconds.
• the expanded PTFE/PPX-AF4 composite article was formed of a first layer of expanded PPX-AF4, a layer of expanded PTFE, and a second layer of expanded PPX-AF4.
• the expanded PTFE/PPX-AF4 composite article was removed from the oven and allowed to cool to room temperature under restraint of the biaxial batch expander grips. After cooling, the expanded PTFE/PPX-AF4 composite article (i.e., co-expanded PTFE/PPX-AF4 film) was removed from the grips.
• FIG, 16 shows a scanning electron micrograph (SEW) of the cross- section of the co-expanded PTFE/PPX-AF4 composite article taken at 5Q0x magnification.
• SEW scanning electron micrograph
• FIG, 16 illustrates the first tight microstructure (80) (first expanded PPX-AF4 film), the open microstructure (90) (ePTFE membrane), and the second tight microstructure (100) (second expanded PPX-AF4 film) of the expanded composite article on a carbon tape SEM mount (110).
• the Gurley number of the expanded PPX-AF4 polymer article was determined to be 137.5 seconds
• a layer of PPX-AF4 was removed from one side of the co-expanded PPX-AF4 article of Example 15 to form an expanded PTFE/PPX-AF4 composite article formed of a layer of expanded PPX-AF4 and a layer of expanded PTFE (having a tight/open microstructure).
• FIG, 17 shows a scanning electron micrograph (SEM) of the cross- section of the co-expanded PTFE/PPX-AF4 composite article taken at 500x magnification
• FIG. 17 illustrates the tight microstructure of the expanded PPX-AF4 film (120) and the open microstructure of the ePTFE (130).
• Gurley number of the porous PTFE/PPX-AF4 composite article was determined to be 79.0 seconds.

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