# US 7,611,565 B1 · Device for hydrogen separation and method

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- Number: US 7,611,565 B1
- Document ID: US7611565B1
- Status: Granted
- Kind: B1
- Application number: 11/581,981
- Filed: 2006-10-16
- Granted: 2009-11-03
- Earliest claimed: 2005-10-20
- Assignees: Los Alamos National Security, LLC
- Inventors: Stephen N. Paglieri; Iver E. Anderson; Robert L. Terpstra
- Web page: https://patentgrep.com/patent/US7611565B1

## CPC

- B01D 53/228: {characterised by specific membranes}
- B01D 69/106: {Membranes in the pores of a support, e.g. polymerized in the pores or voids}
- B01D 69/108: {Inorganic support material}
- C01B 3/505: Membranes containing palladium
- C01B 2203/0405: Purification by membrane separation
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}

## Abstract

A device for hydrogen separation has a porous support and hydrogen separation material on the support. The support is prepared by heat treatment of metal microparticles, preferably of iron-based or nickel-based alloys that also include aluminum and/or yttrium. The hydrogen separation material is then deposited on the support. Preferred hydrogen separation materials include metals such as palladium, alloys, platinum, refractory metals, and alloys.

## Claims

### Claim 1

A device for separating hydrogen from other materials, comprising:
a porous substrate of metal microparticles of an alloy of chromium, aluminum, and iron, the metal microparticles being coated with an outer atomic diffusion barrier layer comprising aluminum oxide that is substantially incapable of hydrogen reduction the porous substrate prepared by sintering said metal microparticles until said outer atomic diffusion barrier layer forms on the surface of the microparticles; and
hydrogen separation material on the diffusion barrier layer of the support structure.

### Claim 2 (depends on 1)

The device of claim 1, wherein said porous substrate of metal microparticles comprises microparticles of Fe-16Al-2Cr.

### Claim 3 (depends on 1)

The device of claim 1, wherein said hydrogen separation material is comprised of palladium or alloys of palladium.

### Claim 4 (depends on 1)

The device of claim 1, wherein the metal microparticles comprise spherical microparticles.

### Claim 5 (depends on 1)

The device of claim 1, wherein said porous substrate comprises pore sizes in a range of from about 0.05 micrometers to about 0.5 micrometers.

### Claim 6 (depends on 1)

The device of claim 1, wherein said porous substrate comprises pore sizes in a range of from about 0.1 micrometers to about 0.3 micrometers.

### Claim 7

A method for making a device for separating hydrogen from a gaseous mixture, comprising:
forming a porous support structure from microparticles of an alloy of chromium, aluminum, and iron, said porous support being formed by sintering the microparticles until an outer diffusion barrier layer comprising aluminum oxide that is substantially incapable of hydrogen reduction forms on the alloy microparticles; and
depositing hydrogen separation material on the diffusion barrier layer of the support structure.

### Claim 8 (depends on 7)

The method of claim 7, wherein the microparticles used for forming the support structure comprise spherical microparticles.

### Claim 9 (depends on 7)

The method of claim 7, wherein the alloy is Fe-16Al-2Cr.

### Claim 10 (depends on 7)

The method of claim 7, wherein the step of forming said support structure is performed by sintering the microparticles together so that a support structure having pore sizes in a range of from about 0.05 micrometers to about 0.15 micrometers is formed.

### Claim 11 (depends on 7)

The method of claim 7, wherein the metal microparticles are applied onto a macroporous membrane prior to sintering.

### Claim 12 (depends on 9)

The method of claim 9, wherein the sintering is at a temperature of approximately 975° C. for approximately 4 hours.

### Claim 13 (depends on 12)

The method of claim 12, wherein the hydrogen separation material is comprised of palladium or alloys of palladium.

### Claim 14 (depends on 7)

The method of claim 7, where the step of depositing the hydrogen separation material is by a technique selected from the group consisting of electroless plating, electroplating, chemical vapor deposition, physical vapor deposition, ion exchange, impregnation and reduction, and combinations thereof.

### Claim 15

A method for separating hydrogen, comprising:
forming a porous support structure by sintering metal microparticles of an alloy of chromium, aluminum, and iron wherein the sintering results in an outer diffusion barrier layer comprising aluminum oxide on the microparticles that is substantially incapable of hydrogen reduction;
depositing hydrogen separating material on the diffusion barrier layer, thereby forming a device for separating hydrogen; and
using the device to separate hydrogen.

### Claim 16 (depends on 15)

The method of claim 15, wherein the hydrogen separating material is comprised of palladium or alloys of palladium.

### Claim 17 (depends on 15)

The method of claim 15, wherein the porous support structure further comprises yttrium.

### Claim 18 (depends on 15)

The method of claim 15, wherein the microparticles used for forming the support structure comprise spherical microparticles.