# US 10,865,112 B2 · Modified track-etched substrates for composite graphene membranes

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- Number: US 10,865,112 B2
- Document ID: US10865112B2
- Status: Granted
- Kind: B2
- Application number: 16/218,859
- Filed: 2018-12-13
- Published: 2020-06-18
- Granted: 2020-12-15
- Earliest claimed: 2018-12-13
- Assignees: Lockheed Martin Corporation
- Applicants: Lockheed Martin Corporation
- Inventors: Scott E. Heise; Han Liu; Jacob L. Swett; Michael J. Hiltabidle
- Web page: https://patentgrep.com/patent/US10865112B2

## CPC

- B32B 1/00: Layered products having a non-planar shape
- C01B 32/194: After-treatment
- B32B 3/26: characterised by a particular shape of the outline of the cross-section of a continuous layer; characterised by a layer with cavities or internal voids {(foam layer B32B5/18; layer of synthetic resin characterised by fillers that create voids or cavities B32B27/205); characterised by an apertured layer}
- B32B 3/28: characterised by a layer comprising a deformed thin sheet {, i.e. the layer having its entire thickness deformed out of the plane}, e.g. corrugated, crumpled (B32B29/08 takes precedence)
- B32B 7/12: using interposed adhesives or interposed materials with bonding properties
- B32B 9/005: {comprising one layer of ceramic material, e.g. porcelain, ceramic tile (layered products with at least two ceramic layers composed mainly of ceramic B32B18/00)}
- B32B 9/041: {of metal}
- B32B 9/045: {of synthetic resin}
- B32B 15/043: {of metal (B32B15/01 takes precedence)}
- B32B 15/08: of synthetic resin
- B32B 15/082: comprising vinyl resins; comprising acrylic resins
- B32B 15/085: comprising polyolefins
- B32B 15/088: comprising polyamides
- B32B 15/09: comprising polyesters
- B32B 15/095: comprising polyurethanes
- B32B 23/04: comprising such {cellulosic plastic} substance as the main or only constituent of a layer, {which is} next to another layer of {the same or of} a {different material (next to a glass layer B32B17/08)}
- B32B 23/042: {of metal}
- B32B 23/08: of synthetic resin
- B32B 23/20: comprising esters
- B32B 25/00: Layered products comprising {a layer of} natural or synthetic rubber {(fibrous or filamentary layer made of a natural or synthetic rubber B32B5/02; particulate layer made of a natural or synthetic rubber B32B5/16; foamed layer made of a natural or synthetic rubber B32B5/18)}
- B32B 27/08: of synthetic resin
- B32B 27/281: {comprising polyimides}
- B32B 27/283: {comprising polysiloxanes}
- B32B 27/285: {comprising polyethers}
- B32B 27/286: {comprising polysulphones; polysulfides}
- B32B 27/288: {comprising polyketones}
- B32B 27/304: {comprising vinyl halide (co)polymers, e.g. PVC, PVDC, PVF, PVDF}
- B32B 27/308: {comprising acrylic (co)polymers}
- B32B 27/32: comprising polyolefins {(comprising vinyl (co)polymers or acrylic (co)polymers B32B27/30)}
- B32B 27/322: {comprising halogenated polyolefins, e.g. PTFE}
- B32B 27/34: comprising polyamides
- B32B 27/36: comprising polyesters
- B32B 27/365: {comprising polycarbonates}
- B32B 27/40: comprising polyurethanes
- B32B 2255/20: Inorganic coating
- B32B 2270/00: Resin or rubber layer containing a blend of at least two different polymers
- B32B 2307/706: Anisotropic
- B32B 2307/732: Dimensional properties
- B32B 2535/00: Medical equipment, e.g. bandage, prostheses or catheter
- C01B 2204/04: Specific amount of layers or specific thickness
- B32B: LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}

## Abstract

Modified substrates are provided having nano- or microscale wells, tracks, channels, pores or perforations. Also provided are methods of making the same.

## Claims

### Claim 1

A modified substrate comprising:
a first face and an opposite facing second face 3 to 30 μm from each other defining a thickness;
a first plurality of track-etched pores through the substrate; and
a well in the first face of the substrate, wherein the well is from 100 to 1,000 μm in diameter, and wherein the well comprises a bottom surface that is 1 to 10 μm from the second face of the substrate, and wherein the pores have an average diameter between 10-2,000 nm.

### Claim 2 (depends on 1)

The modified substrate of claim 1, wherein the first plurality of pores comprises about 1×105 to 1×1011 pores per cm2 of substrate.

### Claim 3 (depends on 2)

The modified substrate of claim 2, wherein the first plurality of pores comprises about 1×107 to 1×1010 pores per cm2 of substrate and has an average pore diameter between 100-2,000 nm.

### Claim 4 (depends on 2)

The modified substrate of claim 2, wherein the first plurality of pores comprises about 1×105 to 1×108 pores per cm2 of substrate.

### Claim 5 (depends on 1)

The modified substrate of claim 1, wherein the second face comprises a coating of a two dimensional material or multiple layers thereof, wherein the two dimensional material is selected from graphene, graphene platelets, black phosphorous, hafnium dioxide, molybdenum disulfide, molybdenum diselenide, carbide, a carbon nanomembrane (CNM), carbon nanotubes (CNT), graphyne, borophene, germanene, silicone, Si2BN, stanine, phosphorene, bismuthene, molybdenite, palladium, rhodium, Pb/Sn alloy, Pb/Bi alloy, aerographite, aerogel, nanogel, carbon nanofoam, amorphous carbon and hydrocarbons, hexagonal boron nitride, borocarbonitride, germanane, transition metal dichalcogenide, or any combination thereof.

### Claim 6 (depends on 5)

The modified substrate of claim 5, wherein the two dimensional material or multiple layers thereof comprises graphene.

### Claim 7 (depends on 5)

The modified substrate of claim 5, wherein the two dimensional material comprises a plurality of perforations therethrough.

### Claim 8 (depends on 5)

The modified substrate of claim 5, further comprising an intermediate layer comprising electrospun nanofibers or carbon nanotubes, between the second face and the two dimensional material.

### Claim 9 (depends on 1)

The modified substrate of claim 1, wherein the substrate comprises polysulfones, polyurethane, polymethylmethacrylate (PMMA), polyglycolid acid (PGA), polylactic acid (PLA), polyethylene glycol (PEG), polylactic-co-glycolic acid (PLGA), polyamides, polyimides, polypropylene, polyethersulfones (PES), polyvinylidine fluoride (PVDF), cellulose acetate, polyethylene, polyethylene terephthalate (PET), polypropylene, polycarbonate, polytetrafluoroethylene (PTFE), polyvinylchloride (PVC), polyether ether ketone (PEEK), polycaprolactone, polydimethylsiloxane (PDMS), block co-polymers of any thereof, or mixtures of any two or more thereof.

### Claim 10 (depends on 1)

The modified substrate of claim 1, further comprising nanowires or a support mesh embedded therein.

### Claim 11 (depends on 1)

The modified substrate of claim 1, wherein the modified substrate is comprised of two or more materials anisotropically arranged or present in a gradient.

### Claim 12 (depends on 1)

The modified substrate of claim 1, wherein the first plurality of pores comprises pores having a diameter at the first face that is between 5-20% greater than their diameter at the second face.

### Claim 13 (depends on 1)

The modified substrate of claim 1, further comprising a second plurality of pores therethrough, wherein the second plurality of pores comprises pores having an average diameter of up to 50% the average diameter of the pores of the first plurality of pores and wherein the second plurality of pores is comprised of 1×107 to 1×1013 pores per cm2 of substrate.

### Claim 14 (depends on 13)

The modified substrate of claim 13, wherein the pores of the first and/or second pluralities of pores comprise a diameter at the first face that is between 5-20% greater than their diameter at the second face.

### Claim 15 (depends on 13)

The modified substrate of claim 13, wherein the modified substrate has a porosity of between 20-50%.

### Claim 16 (depends on 15)

The modified substrate of claim 15, wherein the porosity is between 35% to 50%.

### Claim 17 (depends on 1)

The modified substrate of claim 1, wherein the first face further comprises functionalization, texturing, additional etching, plasma treatment, or a coating.

### Claim 18 (depends on 17)

The modified substrate of claim 17, wherein the coating is selected from a hydrogel, non-porous graphene, graphene oxide, carbon nanotubes or electrospun nanofibers.

### Claim 19 (depends on 1)

The modified substrate of claim 1, wherein all of the bottom surface is 1 to 10 μm from the second face of the substrate.

### Claim 20

A modified substrate comprising:
a first face and an opposite facing second face 6 to 30 μm from each other defining a thickness;
a first plurality of pores through the substrate, comprising about 1×105 to 1×1011 pores per cm2 of substrate and pores having an average diameter between 10-10,000 nm; and
a second plurality of pores through the substrate, comprising pores having an average diameter of 1% to 50% the average diameter of the pores of the first plurality of pores, wherein the second plurality of pores is comprised of 1×107 to 1×1013 pores per cm2 of substrate,
wherein the second face comprises a coating of a two dimensional material or multiple layers thereof, wherein the two dimensional material is selected from graphene, graphene platelets, black phosphorous, hafnium dioxide, molybdenum disulfide, molybdenum diselenide, carbide, a carbon nanomembrane (CNM), a carbon nanotube (CNT), amorphous carbon and hydrocarbons, graphyne, borophene, germanene, silicone, Si2BN, stanine, phosphorene, bismuthene, molybdenite, palladium, rhodium, Pb/Sn alloy, Pb/Bi alloy, aerographite, aerogel, nanogel, carbon nanofoam, hexagonal boron nitride, borocarbonitride, germanane, transition metal dichalcogenide, or any combination thereof.

### Claim 21 (depends on 20)

The modified substrate of claim 20, wherein the pores of the first and/or second pluralities of pores have a diameter at the first face that is between 5-20% greater than their diameter at the second face.

### Claim 22 (depends on 20)

The modified substrate of claim 20, wherein the porosity is between 35% to 50%.

### Claim 23 (depends on 20)

The modified substrate of claim 20, wherein the two dimensional material comprises graphene.

### Claim 24 (depends on 20)

The modified substrate of claim 20, wherein the two dimensional material comprises a plurality of perforations therethrough.

### Claim 25 (depends on 20)

The modified substrate of claim 20, further comprising an intermediate layer comprising electrospun nanofibers between the second face and the two dimensional material.

### Claim 26 (depends on 20)

The modified substrate of claim 20, wherein the substrate comprises polysulfones, polyurethane, polymethylmethacrylate (PMMA), polyglycolid acid (PGA), polylactic acid (PLA), polyethylene glycol (PEG), polylactic-co-glycolic acid (PLGA), polyamides, polyimides, polypropylene, polyethersulfones (PES), polyvinylidine fluoride (PVDF), cellulose acetate, polyethylene, polyethylene terephthalate (PET), polypropylene, polycarbonate, polytetrafluoroethylene (PTFE), polyvinylchloride (PVC), polyether ether ketone (PEEK), polycaprolactone, polydimethylsiloxane (PDMS), block co-polymers of any thereof, or mixtures of any two or more thereof.

### Claim 27 (depends on 20)

The modified substrate of claim 20, further comprising nanowires or a support mesh embedded therein.