The present invention is generally directed to a porous membrane. In particular, the present invention is directed to a porous expanded polytetrafluoroethylene membrane having improved properties and made from multiple extrudates.
Membranes made from expanded polytetrafluoroethylene (ePTFE) are known. Such known membranes are used in many applications because of their chemical inertness. Exemplary applications for ePTFE membrane use include waterproof and breathable garments, fluid filtration, medical implantation and venting.
The membranes are typically made to attain a particular property such as air permeability or moisture vapor transmission. The desired property can often be attained by producing a membrane with a predetermined pore size, thickness and/or unit weight. Previous attempts at improving membrane properties have been to coat the membrane with a polymer such as polyurethane or to use multiple membranes or intermediate membrane components to provide a composite membrane. Despite this ability to modify the ultimate resultant membrane, there is still a need to improve the membrane.
One aspect of the invention is a membrane having at least one improved property, such as increased strength or durability. The membrane comprises a sheet of expanded polytetrafluoroethylene. The sheet is porous and has a gas permeability of at least 0.1 CFM according to ASTM D737. The sheet has an average Mullen Hydrostatic Burst pressure in the range of 135 psi to 175 psi according to ASTM D751.
Another aspect of the invention is a membrane that comprises a sheet of expanded polytetrafluoroethylene. The sheet includes a first extrudate made from a first PTFE fine powder resin mixed with processing lubricant at a first lube rate. A second extrudate is made from the first PTFE fine powder resin mixed with processing lubricant at the first lube rate. The first and second extrudates combined into an integrated tape structure that is bi-axially stretched. The sheet is porous and has a gas permeability of at least 0.1 CFM according to ASTM D737. The sheet has an average Mullen Hydrostatic Burst pressure in the range of 135 psi to 175 psi according to ASTM D751.
Another aspect of the invention is a method of making a membrane. The method comprises the steps of providing a first extrudate made from a first PTFE fine powder resin mixed with processing lubricant at a first tube rate. A second extrudate is provided and made from the first PTFE fine powder resin mixed with processing lubricant at the first lube rate. The first and second extrudates are overlaid. The overlaid first and second extrudates are calendered into an integrated tape. The integrated tape is stretched in the machine direction. The integrated tape is stretched in the transverse direction to provide a porous sheet that has a gas permeability of at least 0.1 CFM according to ASTM D737 and an average Mullen Hydrostatic Burst pressure in the range of 135 psi to 175 psi according to ASTM D751.
Further features of the invention will become apparent to those skilled in the art to which the invention relates from reading the following description with reference to the accompanying drawings, in which:
An improved membrane 20 (
The resultant sheet 22 of membrane 20 is porous, and preferably microporous, with a three-dimensional matrix or lattice type structure of numerous nodes 62 interconnected by numerous fibrils 64. The material that the sheet 22 is made from expanded polytetrafluoroethylene (ePTFE) that may or may not be sintered.
Surfaces of the nodes 62 and fibrils 64 define numerous interconnecting pores that extend completely through the sheet 22 between opposite major side surfaces of the membrane in a tortuous path. Preferably, the average size of the pores in the sheet 22 is sufficient to be deemed microporous, but any pore size may be used in the present invention. A suitable average size for the pores in the sheet 22 may be in the range of 0.01 to 1.0 micron, and preferably in the range of 0.01 to 0.25 micron and most preferably in the range of 0.01 to 0.10 micron. This porosity enables the sheet 22 to be permeable. For example, the sheet has an air permeability, measured according to ASTM D737 test method, in the range of about 0.10 CFM to 0.30 CFM.
The sheet 22 is made by mixing of polytetrafluoroethylene (PTFE) fine powder and lubricant in a mixer 100 (
The mixture of lubricant and PTFE fine powder resin is introduced into a preformer 120. The preformer 120 mechanically compresses the mixture of lubricant and PTFE fine powder resin into a billet (not shown). The billet has an elongated cylindrical shape that can have any suitable diameter, such as in the range of about 2 inches to 6 inches. The billet may be stored at this stage to allow the lubricant to better penetrate into the PTFE fine powder resin.
The billet is placed in an extruder 140. The extruder 140 is a press that forces the mixture of lubricant and PTFE fine powder resin of the billet through a die of the extruder to yield the extrudate 24, 26. During the extrusion process, fibrils are formed as raw dispersion particles of the PTFE fine powder resin move passed one another. The extrudates 24, 26 have a predetermined thickness, dependent on the die configuration, in the range of about 0.035 inch to 0.045 inch and preferably about 0.040 inch. By way of example, according to one aspect of the invention the extrudates 24, 26 are substantially identical in thickness and lube rate. The extrudates may be wound up on a roll 142 for temporary storage.
The extrudates 24, 26 are trained off their respective rolls 142 and directed into a calender 160 (
The calender 160 forms the integrated tape 40 from the extrudates 24, 26. The first and second extrudates 24, 26 are forced into engagement with one another because the gap between the rollers 162, 164 is less than the combined thicknesses of the extrudates 24, 26. The gap is in the range of about 0.010 inch to 0.030 inch and preferably about 0.020 inch. The rollers 162, 164 are metal and each heated to a temperature in the range of about 160° F. to 320° F., depending on the number and thickness of the extrudates 24, 26 used. The thickness of the integrated tape 40 is preferably in the range of about 0.010 inch to 0.030 inch and preferably about 0.020 inch.
The first and second extrudates 24, 26 are combined into the integrated tape structure 40 by mechanically interlocking the nodes 62 and fibrils 64 making up the first and second extrudates. That is, during the calender operation, a portion of the first extrudate 24 is forced into a portion of the second extrudate 26. This provides a relatively strong integrated tape structure 40 that enables other desirable improved properties of the finished sheet 22 of membrane 20.
The integrated tape structure 40 is trained over a series of heated drying rollers 180 (
The integrated tape structure 40 is “expanded” or stretched in at least one and preferably two (bi-axially) directions to form the finished sheet 22 of membrane 20. “Expanded” is intended to mean sufficiently stretched beyond the elastic limit of the membrane material to introduce permanent set or elongation to the fibrils 64.
The integrated tape structure 40 is directed to a machine direction MD stretcher 200. The machine direction stretcher 200 has a first roller 202 that is rotating at a first speed. The machine direction stretcher 200 has a second roller 204 that is rotating at a second speed greater than the first speed of the first roller 202. The rollers 202, 204 are heated in the range of about 260° F. to 300° F. and preferably about 280° F. The surface speed differential of the second roller 204 rotating faster than the surface speed of the first roller 202 determines the ratio of machine direction MD stretch. The machine direction MD stretch ratio, according to one aspect of the invention, is in the range of about 1.0 to 6.0 and preferably in the range of about 2.0 to 3.5.
The integrated tape structure 40 is directed to a transverse or cross direction XD stretcher 220. The integrated tape structure 40 is clamped at its laterally opposite edges by parts of the cross direction XD stretcher 220. The integrated tape structure 40 is stretched in a second direction, substantially orthogonal to the machine direction MD a predetermined amount to form the sheet 22. The integrated tape structure 40 is stretched in the cross direction XD direction in the range of about 8 to 12 times its original cross direction dimension (width) and preferably about 10 times. The integrated tape structure 40 is stretched when exposed to elevated temperatures in the range of about 500° F. to 600° F. and preferably about 550° F.
The sheet 22 is preferably heated or “sintered” to reduce and minimize residual stress in the membrane material. The sheet 22 is preferably heated in the cross direction stretcher 220 by exposure to elevated temperatures in the range of about 700° F. to 750° F. and preferably about 730° F. However, the sheet 22 may be unsintered or partially sintered as is appropriate for the contemplated use of the membrane 20. The sheet 22 of the membrane 20 is the rolled onto roll 222.
The sheet 22 of membrane 20, according to one aspect of the invention, was tested against known membranes. Results of the testing are presented in the table below. Samples 1-5 are known ePTFE membranes only made from a single extrudate. Sample 6 is a known ePTFE membrane made from a single extrudate and coated with a polyurethane material. Samples 7-9 are sheets 22 of membrane 20 made according to one aspect of the invention. The sheet 22 of membrane 20, according to one aspect of the invention, has significantly improved desirable properties, such as Mullen Hydrostatic, which is indicative of strength and durability. The sheet 22 has an average Mullen Hydrostatic Burst pressure in the range of 135 psi to 175 psi according to ASTM D751 while retaining air permeability and preferably in the range of 135 psi to 175 psi.
From the above description of at least one aspect of the invention, those skilled in the art will perceive improvements, changes and modifications. Such improvements, changes and modifications within the skill of the art are intended to be covered by the appended claims.